MasterGC Operating Manual Rev.4.0

A SCENT
OF
FUTURE
MasterGC Gas Chromatograph

MasterAS Liquid Autosampler
Operating Manual
rev. 4.0
Edition
MasterGC - Operating manual
Rev. 4.0 (2014) from rev 20141003
Warnings
The information contained in this document can be updated by DANI Instruments Spa at any
time without prior warning.
DANI Instruments Spa shall not be held liable for any errors in this manual or improper use of the
information contained in it or of the instrument.
It is advisable for users to carefully read all the information contained in this manual before
using the instrument.
Safety Information
Refer to Technical Specification – Safety and Regulatory Certifications for applicable Directives
and Reference Standards.
The Master GC has been designed and tested in accordance with safety standards for indoor use.
The Master GC is Equipment Class I, Pollution Degree 2 and Installation Category II, cord
connected.
The Master AS has been designed and tested in accordance with safety standards for indoor use.
The Master AS is Equipment Class III, Pollution Degree 2 and Installation Category II, intended to
be supplied by an external separately approved power supplied.
The Master AS is fixed to Master GC and is not intended to be used as stand-alone instrument.
If the instruments are used in a manner not indicated by the manufacturer, the protection devices
on the equipment could be damaged. If this occurs, disconnect the unit from the electrical power
supply and make sure it cannot be accidently started up.
The instruments should only be serviced by professionally trained personnel. Do not replace
parts or make modifications on the instruments unless authorization. Users cannot replace fuses.
Always disconnect the power supply cord before lifting the lid or removing the covers.
Master AS has parts that move during the operation. Keep your hands away from moving parts
during operation.
The instruments are not intended to be moved when in use.
Only the smooth external surfaces of the instrument should be cleaned. Always switch off the
instrument, remove the power supply cable from the outlet and let any hot parts cool down. Only
use a slightly damp cloth. Do not use alcohol or other solvents.
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Safety symbols
The warnings in the manual and on the instruments must be observed both during operating phases
and when servicing. Failure to observe these rules violates the design and instruments use safety
standards.
DANI Instruments S.p.a bears no liability for user failure to observe these rules.
Attention! Warns of a condition or possible situation which could cause damage or harm the user.
Warning Warns of a condition or possible situation which could damage or destroy the product or the operator’s
work
Indicates a grounded terminal.
This symbol indicates a hot surface
Attention! Refer to attached documentation
Indicates hazardous voltages
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Table of Contents
MasterGC Overview 2
Oven 2
Display 3
Injectors and Detectors Compartment 3
Pneumatic compartments 3
Electronic compartment 4
Connection/communication compartment 4
Master GC User Interface 5
Status Bar 5
Menu 6
Status 7
Time Clock and Date 8
Desktop 9
Tool Bar 11
How to enter a value and select a parameter 12
Oven 15
Oven temperature 17
Setting the maximum temperature 17
Setting the oven temperature (Rates) 17
Maximum rates 19
Oven fan (General) 19
Oven Fast Cooling 20
Conditioning time (General) 20
Cryogenic system (Cryo) 20
GCxGC Modulator (General) 21
Installing the columns 24
Packed columns 24
Nuts and ferrules 24
Nuts 24
Ferrules 25
Packed column installation 26
Capillary columns 26
Positioning the column 26
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Preparing the column 27
Fused silica capillary column 27
Glass capillary columns 27
Nuts and ferrules 27
Nuts 27
Ferrules 27
Assembling the glass liner 29
Split/splitless injector 29
PTV injector 30
Installation of capillary column 32
Installation of the column at the injector 32
Installation of the column in the Flame Ionization Detector 34
Installation of the column in the Electron Capture Detector 34
Installation of the column in the Photoionization Detector 35
Installation of the column in the Nitrogen - Phosphorus Detector 35
Installation of the column in the Thermal Conductivity Detector 35
Installation of the column in the Flame Photometric Detector 36
Leak testing the pneumatic circuit 36
Conditioning the columns 36
Introduction systems 37
Description 37
Pneumatic circuit 38
Adapter for wide-bore capillary column 39
Injector temperature (Temp) 40
Carrier Gas Control (press/flow and column) 40
Split/splitless injector 42
Description 42
Injector temperature 44
Carrier Gas Control (Press/flow and Column) 45
Injection techniques 46
Manual injection (Double Start) 48
Purge flow rate 51
PTV Injector (Programmed Temperature Vaporizer) 54

Description 54
Injector temperature (Temp) 55
Cryogenic system (Cryo) 55
Carrier Gas Control (Press/Flow and Column) 57
Introduction techniques (Split) 58
Manual injection (Double Start): 62
Splitless injection 62
Solvent split injection 63
Pulsed introduction 65
Purge flow rate 66
Gas saving 66
Introducing the sample 67
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On Column – PTV 68
How to install the column 68
On column – PTV Injector: user interface 69
Injector maintenance 70
Cleaning the precolumn 70
Preparing the precolumn 70
Precolumn for Split/splitless injector 70
Precolumn for the PTV injector 71
Precolumn for the PTV injector with adsorbent material 72
Procedure for silanization of the precolumns 73
Conditioning the split line filter 73
Septa 74
Washing procedure for silicone septa 74
Procedure to close the Split/Splitless Septum holder 75
Split/Splitless injector cleaning procedure 75
Detectors 77
Flame Ionization Detector FID 86.10 77

Introduction 77
Description 78
The base body 78
The detector head 79
The control unit 79
Detector temperature 80
Setting the temperature (“Temp” page) 80
Indication temperature (“Status” page) 81
Regulating the gas flow rates 81
Setting the flow rates (“Flows” page) 82
Visualizing gas flows (“Status” page) 82
Flame 82
Auto Ignition 83
Electron Capture Detector ECD 86.10 87

Introduction 87
Sensitivity and selectivity 90
Carrier gas and auxiliary gas 92
Setting the flow rate (“Flows” page) 92
Temperature 94
Current 96
Signal 96
Digital acquisition rate 96
Cleaning and conditioning the system 98
Switching on the detector 99
Thermal Conductivity Detector TCD 86.40 101

Introduction 101
Description 102
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The main body and heating unit 102
The external cover 103
The control unit 105
Response 105
Filament current 106
Carrier and auxiliary gas 106
Carrier and auxiliary gas flow rate 107
Temperature 108
Temperature 109
Filaments 110
Signal 110
Selecting the RANGE level 110
Graphic 112
Switching on 112
Nitrogen-Phosphorous Detector “Blos” 114

Introduction 114
Description 115
Sensitivity and selectivity 117
Effect of gas flow rates 117
Voltage to the bead 118
Temperature 118
Regulating the gas flow rates 120
Detector functioning 121
Graphic 123
Flame Photometric Detector FPD 86.72 124

Introduction 124
Description 125
The base body 125
Gas flow rates 127
The photomultiplier PMP 129
Sulphur quenching 131
Igniting the flame 132
Signal 133
Micro-Thermal Conductivity Detector µTCD 135

Introduction 135
Description 136
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The detector cell and heater block 136
The control units 136
Configuration 137
Differential mode 137
Single filament mode 138
Carrier and auxiliary gas 139
Carrier gas flow rate 140
Temperature 140
Filaments 142
Single filament mode 142
Functioning 145
Signal 146
PhotoIonization Detector PID 86.90 148

Introduction 148
Description 149
The base body 149
Detector head 150
Temperature 151
Auxiliary gas 152
Setting the flow rate (“Flows” page) 152
Visualizing gas flow (“Status” page) 153
Lamp 153
Switching on the detector 154
Signal 154
Graphic 155
Auxiliary temps and gases 157
Auxiliary temperatures 157

Auxiliary gases 158
Method 160
How to create a method 160
Method Sequence 164
Timed events 165

Clock time events 165
Method events 167
Status 169
Instrument condition 169

Stand by/Prep run 169
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Ready 169
Iso, Rate 170
Cooling 170
Waiting 170
Conditioning 170
Control of analysis 171

Start of analysis 171
End of analysis 171
Set up 173
Com 173
Activation code 173
Communication pipe 174
Other 177
AS 180
How to configure an external sampler 180
Lock/Unlock 180
How to configure a cryogenic system for PTV injector 181
Maintenance 182
Touch screen calibration 182
Counters 183
Diagnostics 185
Diagnostic 185
Alarms 186
Leak test 193
Master AS 195
Description 195
Syringe block 196
The electrical connections 196
Set up 197
Vial & Syringe 197
Solvent&Waste 199
AS parameters 199
Sampling mode (Inj. Mode) 199
Sample 199
Air Plug 200
Solvent Plug 201
Internal Standard 202
Sample Handling 205
Solvent Washing 206
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Injector 207
AS Sequence 208
How to create an AS sequence 208
How to start an AS sequence 210
How to stop a sequence 210
AS status 211
Missing vials 211
Maintenance 213
Syringe Cleaning 213
How to install the syringe 214
How to align the MasterAS 214

Alignment on the TRAY without the syringe (Z Axis) 214
Alignment on the Injector without the syringe 215
Alignment on the TRAY with the syringe (X-Y axes) 215
Checking the injector 216
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Technical Specifications
Master GC
DIMENSIONS
Size 570x500x590 mm (W x H x D)
Weight 60Kg
ENVIRONMENTAL CONDITIONS
Operating temperature 0–40°C

Operating humidity 5-95%
Altitude: up to 2000 m
LINE VOLTAGE REQUIREMENTS 240Vac (±10% max), 50-60 Hz, 3400 VA
HEATED ZONES
Independent heated zones, not 3 injectors, 3 detectors, 2 auxiliary temps (max temperature
including oven 450°C)
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COLUMN OVEN
Dimensions 280x280x160 mm (W x H x D)
Operating temperature 5°C above ambient to 500°C

-50°C to 500°C with liquid CO2 cryogenic cooling option -
-100°C to 500°C with liquid N2 cryogenic cooling option
Temperature setpoint resolution 1°C
Thermal accuracy ± 0.1°C
Thermal stability ± 0.1°C
Temperature programming 25 ramps, 26 isotherms, 0.1 to 140.0°C/min (see Table 1)
Typical cool-down rate 300°C to 50°C in 4 min
Isothermal time 0.00 to 999.00 min, 0.01 min setpoint resolution
Temperature 240V line voltage

range (°C) rates (°C/min)
30 to 70 140
70 to 115 95
115 to 175 70
175 to 300 50
300 to 450 35
450 to 500 30
Table 1 – Typical Master GC Oven Ramp Rates

*Results obtained with line voltage maintained constant
PNEUMATIC CONTROL
Pressure range 0-120 psi
Carrier gas max total flow 1000 mL/min (He)
Pressure/flow programming Constant or programmed flow, constant or programmed

pressure, constant linear velocity Flow programming: 25
ramps/26 cost. flows; pressure programming: 25
ramps/26 isobars Pressure resolution: 0.001 bar
Atmospheric pressure and temperature

compensation
INJECTORS
Injectors Packed (PK), split/splitless (SL/IN), programmable

temperature vaporizer (PTV), gas sampling valves
Carrier gas He, N2, H2, Ar, Ar+CH4
Maximum number 3
Max number of PTV/ On column-PTV 2
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PACKED
Suitable for Packed (6 mm, 4 mm, 1/8” o.d.) and wide-bore columns
(0.53 mm i.d., adapter included)
Temperature Up to 450°C, 1°C setpoint resolution
SPLIT/SPLITLESS (SL/IN)
Suitable for Capillary and wide-bore (0.53 mm i.d.) columns
Temperature Up to 450°C, 1°C setpoint resolution
Injection modes Split, splitless
Carrier gas control Digital flow control (DFC)
Split flow and septum purge Included; direct setting of split and purge flow rates and
split ratio
Liner Quartz liner with glass wool
PROGRAMMABLE TEMPERATURE VAPORIZER (PTV)
Suitable for Capillary columns
Temperature 10°C above ambient up to 450°C, 1°C resolution

-50°C to 450°C with liquid CO2 cryogenic cooling option
Temperature programming 25 ramps, 26 isotherms
Heating rate 1 - 999°C/min; 1000°C ballistic
Injection modes Split, splitless, solvent split
split ratio
Liner Quartz liner with glass wool.

Special adsorbent for enrichment technique (with
solvent split injection mode) available as option
ON COLUMN-PTV
(Currently available on SimDis System only)
Temperature 10°C above ambient up to 450°C, 1°C resolution

-50°C to 450°C with liquid CO2 cryogenic cooling option
Temperature programming 25 ramps, 26 isotherms
Heating rate 1 - 999°C/min; 1000°C ballistic
Injection modes Split, splitless, solvent split
split ratio
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DETECTORS
Detectors FID flame ionization detector

NPD nitrogen and phosphorous detector
ECD electron capture detector
PID photo ionization detector
TCD thermal conductivity detector
mTCD micro thermal conductivity detector
FPD flame photometric detector
Maximum number of detectors 3
Maximum number of TCD 2
Maximum number of µTCD 1 complete, 1 with a single Master channel working
Output signals Digital and analog outputs (0-1V, 0-10V)
FID (Flame Ionization Detector)
Suitable for Packed, wide-bore and capillary columns
Temperature Up to 450°C, 1°C resolution

7
Linear dynamic range >10
Minimum Detectable Level <1.6 pg Carbon/sec (as C14)
Flame out detection Automatic re-ignition
NPD Blos

5
Linear dynamic range > 10
Selectivity 63000 gN/gC as octadecane

240000 gP/gC as octadecane
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ECD (Electron Capture Detector)

4
Linear dynamic range >10 lindane
Minimum Detectable Level <6 fg/sec lindane
63
Radioactive source 10 mCi Ni
PID (Photo Ionization Detector)

5
Linear dynamic range >10 with naphthalene
Minimum Detectable Level <0.1 pg naphthalene/mL carrier gas
Ionization lamp 10.2 eV
TCD (Thermal Conductivity Detector)
Suitable for Packed and wide-bore columns

5
Minimum Detectable Level <10 ng hexadecane/mL He (carrier gas)
Configuration Dual filaments (Wheatstone bridge)
Filament protection Standard
mTCD (Micro Thermal Conductivity Detector)
Suitable for Wide-bore and capillary columns
Cell temperature stability ±1°C

3
Minimum Detectable Level <100 pg butane
Configuration 2 filaments, independent or differential operation;

recommended flow rate 1-10 mL/min
FPD (Flame Photometric Detector)
BodyTemperature Up to 450°C, 1°C resolution

3
Linear dynamic range S>10
P>10
Minimum Detectable Level <40 pg sulphur/sec as dodecanethiol<0.4 pg
phosphorous/sec as tributylphosphate
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6
Selectivity >10 gS/gC as isooctane
6
>10 gP/gC as isooctane
Configuration Single or double flame
DATA COMMUNICATION
Remote control Start in; start and ready out (contact relays normally
open)
Communication RS232, LAN, USB
Time events 4 voltage free contacts (contact relays normally open)4

24V outputs
TOUCH SCREEN GRAPHIC USER INTERFACE
Display LCD TFT, 5.7”
Resolution 240x320 pixel
Colors 65,536
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Safety and Regulatory Certification-MasterGC

The Master GC is in compliance with the following European Directives and
Reference Standards:
APPLICABLE EUROPEAN DIRECTIVES

EMC Electromagnetic Compatibility Directive 2004/108/EC
Safety Low Voltage Directive 2006/95/EC
REFERENCE STANDARDS
EMC EN 61326-1: 2006, EN 55011: 2007 + A2: 2007, Class A Group 1
IEC 61326-1: 2005, CISPR 11: 2003 + A2: 2006, Class A Group 1
Safety EN 61010-1: 2010 (3rd edition)
IEC 61010-1: 2010 (3rd edition)
CAN/CSA-C22.2 No 61010.1-04
UL Std. No 61010-1 (2nd edition)
DECLARATION OF CONFORMITY
The Declaration of Conformity is available.
QUALITY SYSTEM
The Master GC is designed and manufactured under a registered ISO 9001 quality system.
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MasterAS
System type XYZ robot
Vial Volume 2 mL (0.1 mL with adapter), 10 mL, 20 mL
Vial capacity 160 (2 mL vials) or 65 (10 or 20 mL vials)
Solvent 5 (10 mL vials)
Waste 5 (10 mL vials)
Syringe 5, 10, 25, 50, 100, 250, 500 µL
Parameter Control Pre injection solvent washing
Post injection solvent washing
Sample/Internal Standard rinse
Sample taking heigh
Injection depth
Syringe strokes before injection
Plunger Injection speed
Viscosity delay
Pre-injection delay
Post-injection delay
Solvent plug volume
Internal standard volume
Smple volume
Air plug volume
Sampling washing 25
Pre-injection solvent washing 25
Post- injection solvent washing 25
Injection per vial 100
Injection port up to 3
Repeatability RDS%<0.5%
User interface MasterGC touch screen graphic user interface
Data Communication 1 RS232 port
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Option 10 and 20 mL vial tray
Electrical supply 24Vdc, 120W
Size 455x750x650 mm (WxHxD)
Wheight 13 Kg
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Safety and Regulatory Certification-MasterAS
The Master AS is in compliance with the following European Directives and Reference
Standards:
APPLICABLE EUROPEAN DIRECTIVES

EMC Electromagnetic Compatibility Directive 2004/108/EC
Safety Low Voltage Directive 2006/95/EC
REFERENCE STANDARDS
EMC EN 61326-1: 2006, EN 55011 Class A Group 1
IEC 61326-1: 2005, CISPR 11 Class A Group 1
Safety EN 61010-1: 2010 (3rd edition)
IEC 61010-1: 2010 (3rd edition)
CAN/CSA-C22.2 No 61010.1-04
UL Std. No 61010-1 (2nd edition)
DECLARATION OF CONFORMITY
The Declaration of Conformity is available.
QUALITY SYSTEM
The Master AS is designed and manufactured under a registered ISO 9001 quality system.
1
MasterGC Overview
The MasterGC consists of six main components, as shown in figure 1:
• oven (1)
• display (2)
• injectors and detectors compartment (3)
• pneumatic compartment (4)
• electronic compartment (5)
• communication compartment (6)
Fig. 1 - Master GC system components
Oven
The gas chromatograph oven provides the housing and heating for the analytical columns.
The air circulation and the oven insulation guarantee a homogeneous, stable and accurate heating of the
column and provide very precise analytical performances.
The MasterGC column oven has fast heating and fast cooling capability.
The oven can operate from temperature below ambient, with a cryogenic cooling system, up to
500 °C maximum temperature.
Refer to Chapter “The Column Oven” for details.

2
Display
The high resolution LCD display and its touch screen functionality constitute the MasterGC user
interface.
All functions, including liquid autosampler programming, can be managed by the MasterGC
display.
The display allows to gain access to every parameter by no more than four touches on the touch
screen.
Refer to Chapter “MasterGC User Interface” for details.
Injectors and Detectors Compartment

The injectors and detectors compartment is located on the top of the column oven.
The injectors are installed on the left side, the detectors on the right side. Up to three injectors and
three detectors can be installed contemporarily. The injectors and detectors positions are
identified as A, B and C starting from the front to the back of the instrument.
The following injectors are available on MasterGC:
• packed injector
• split/splitless injector
• programmable temperature vaporizer (PTV) injector
Up to two PTV injectors can be installed in the same time, in positions B and C.
Refer to Chapter “Introduction Systems” for details.
The following detectors are available on MasterGC:
• FID Flame Ionization Detector

• TCD Thermal Conductivity Detector
• mTCD microThermal Conductivity Detector
• ECD Electron Capture Detector
• NPD NitrogenPhospourous Detector
• FPD Flame Photometric Detector
Up to two TCD and/or mTCD can be instralled in the same time.
Refer to Chapter “Detectors” for details.
Pneumatic compartments
The pneumatic compartment contains the gas control circuit for both injectors and detectors.
Besides, an extra position for the control of up to three auxiliary gas lines is available.
All gas control circuits are electronically controlled.
3
Electronic compartment
The electronic compartment on the right side of the instrument contains the main board, the
detector boards and peripheral control boards. The PTV thermal control is also installed on this
side.
Connection/communication compartment
External electrical/electronic connection are placed on the back of the instrument: the power
supply socket and the main switch are on the lower part.
On the left side, the analog output for the detector signals, the RS232, LAN and USB ports, the
Remote and External Events terminal block are also located.
4
Master GC User Interface
Even if usually coupled with a data system, all Master GC functions, including autosampler
programming, can be managed by the innovative touch screen. The display allows to gain access
to every parameter by no more than four touches on the touch screen.
The display can be divided in three blocks:
• Status Bar
• Desktop
• Tool Bar
Fig. 2- Display
Status Bar
The Status bar is on the bottom of the screen. In this section you can find Menu, Status and Time
Clock.
5
Menu
This section allows to gain access to many functions and to select the submenu (fig. 3). Refer to
each specific chapter for details.
Fig. 3- Menu
Menu and Submenu items are reported in the table below together with the chapter of the manual
where you can find detailed information.
Menu Submenu Reference Chapter
OVEN - Oven
INJECTORS A, B, C Introduction Systems
DETECTORS A, B, C Detectors
AUX - Auxiliary Temps and Gases
TIMED EVENTS - Method
MASTER AS SEQUENCE MasterAS
PARAMETERS MasterAS
MAINTENANCE MasterAS
SET UP MasterAS
TOOLS SET UP Setup
DIAGNOSTIC Diagnostic
MAINTENANCE Maintenance
LOCK/UNLOCK Setup
6
Status
This section is able to show in real time the GC status (see Chapter “Instrument conditions”).
If you press on this bar a window, “Status” will appear. This window consists of three pages: “GC
Status”, “AS Status” and “Alarm”.
When a device is not in the ready status (Oven, Injector, Detector, etc.), the red inscription “Not
Ready” will be visualized (fig. 4): pressing on this message, the status page relative to this parameter
will appear (see fig. 5 and “Status page” in this chapter).
Fig. 4 - GC Status Fig. 5 – Status
When the analysis is running, a blue bar that describes the progress of the analysis, the remaining
time and the actual oven temperature is displayed (fig. 7).
In the page “AS Status” (fig. 6) you can monitor all the steps of the automatic liquid sampler
MasterAS (see “Master AS user interface” in the chapter headed “Master AS”) and, in case of a
7
Fig. 6 -Status Fig. 7 -AS Status during analysis
sample sequence, the number of repetitions, the name of the method in use, the vials and
injector involved in the analysis are also visualized.
In the Alarm page (fig. 8) you can find all the messages concerning problems or advices. To gain
Fig. 8 - Alarm Page
access to this page, press the exclamation mark blinking on the right of the status bar. (see
“Alarm” in the chapter “ Diagnostics”).
Time Clock and Date

This section allows to read the time and date. If you press here, the window “Time & Date” will
8
Fig. 9 - Clock Fig. 10 - Date
appear. Open the page Time (fig. 9) and enter hours, minutes and seconds in the three boxes to set the time.
To set the date, open the page “Date” (fig.10) and select month, day and year.
Desktop
The central portion of the display is the desktop.
Here you can find five buttons that allow to gain access to the corresponding components: Injector,
Detector, Start/Stop, Oven and Lamp.
INJECTORS (see chapter “Introduction systems”)
DETECTORS (see chapter “Detectors”)
OVEN (see chapter “ The column oven”)
LAMP: Pressing this button you can switch on or off the lamp. This
device is equipped with a directional supporting arm and it’s able to
illuminate the oven. (see chapter “MasterGC Overview”).
9
START/STOP: these two buttons are alternatively displayed on the

desktop. When the instrument is out of an analysis, the START button is
displayed. If an analysis is in progress, the STOP button is available.
(see “Control of analysis” in the chapter “Status”).
10
Tool Bar
The Tool Bar (fig. 11) is positioned on the top of the display and consists of three parts:
• the upper left side, where the name of the current method is shown. If you press on this
inscription, the “Manage Methods” and “Method Sequence” pages will be available. (see
the chapter “Method”)
• the upper right side, where the name of the window opened is displayed.
• the lower rows where seven shortcut keys allow to start an application (Start, Stop, “X”
for window closing) or to jump within the windows corresponding to Oven, Injectors,
Detectors, autosampler from left to right respectively.
Fig. 11 - Tool bar
Pressing the button “Injector” or “Detectors” more times you can scroll through all
injectors or detectors configured.
START: (See “Control of analysis” in the chapter “Status”).
STOP:(See “Control of analysis” in the chapter “Status”).
OVEN: In order to set all parameters press this shortcut key.

The “Oven” window consists of four pages (see the chapter “ The
column oven”):
• Rates
• General
• Cryo (if installed)
• Status
11
INJECTORS: In order to set all parameters press this shortcut key. The
“Injectors” window consists of five pages (see the chapter headed
“Introduction systems”):
• Temp
• Press/Flow
• Column
• Split
• Status
DETECTORS: In order to set all parameters press this shortcut key. The
pages in the “Detectors” window depend on the installed detector type. For a
FID there are six pages (see the chapter headed “Detectors”):
• Temp
• Graph
• Flows
• Signal
• Flame
• Status
The last button represents a “X” and allows to close the windows and to come
back to the desktop.
How to enter a value and select a parameter

In order to set a value you have to press on the corresponding box and a numeric keypad will
appear (see fig. 12 ). Digit the value and press OK.
To select a parameter press on the corresponding text box and a drop-down menu will be
visualized (see fig. 13).
12
Fig. 13 – Numeric Keypad Fig. 12 - deopdown
Status page and Ready conditions

A “Status” page (fig. 14) is available for all the devices (Oven, Injectors, Detectors).
In this page you can control the actual value and the set value for the listed parameters.
Besides, you can find the “Ready conditions- Rdy” function.
When all the parameters checked for the “Ready Conditions”, satisfy the set conditions, the
instrument reaches the Ready status (see “Ready” in the chapter headed “Status”).
Fig. 14 - Status page
The parameters available include all the devices that have a temperature regulation, that is
chromatograph oven, injectors, detectors and auxiliary temperatures, all the pressure and flow
regulations on carrier and detector gases.
In the “Default” method, all Ready conditions are active.
To eliminate a parameter from the ready conditions, press on the corresponding check box and
cancel the check.
13
To include a parameter in the “Ready conditions”, press on the corresponding check box to display
the check.
The oven temperature can never be excluded from the Ready conditions.
When a parameter, selected for the “Ready condition”, has not reached its setpoint yet, it will be
visualized in red.
14
Oven
Description
The gas chromatograph oven (fig. 15) provides the housing and heating for the analytical
columns.
Access to the oven is through a door on the front of the instrument.
The door is opened by pushing the latch under the GC on the right hand side of the same.
The internal dimensions of the oven are 280x280x160 mm (wxhxd).
The resistance for heating the air and the air circulation fan (1) are located behind the metal grid
(2), on the rear wall. The oven temperature probe is located on the rear wall (3).
Fig. 15 - MasterGC Oven
On the top of the oven (fig. 15), there are 12 openings: two rows of 3 openings on the left, for
injector terminal fittings(1), and two rows of 3 openings on the right (2), for detector terminal
fittings.
A maximum temperature safety probe for the oven is also in this same area (3).
15
Fig. 16 - Master GC Oven top
Good heat insulation is guaranteed by thermic insulation material inserted both in the hollow wall
and upper surface spaces as well as in the inner part of the access door.
The back panel can be removed for access to the rear of the oven (fig. 17) where the fan motor is
located.
In the same area, two air locks are located which close two openings:
• the upper opening (1), for emission of hot air

• the lower opening (2) for intake of environmental air
The air locks are operated by a stepper motor which regulates their functioning during the oven
cooling phase.
Fig. 17 - MasterGC back
16
Oven temperature
The oven operates at both constant temperature (isotherm) and programmed temperature.
The oven temperature ranges from -100°C (by using a cryogenic cooling system) up to 500 °C,
with 1°C increments. The temperature rates can be set from 0 to 140°C/min with 0.1°C/min
increments.
Oven Temperature Range
Interval (°C) Increment (°C)
temp from +30 to 500 1
with Liquid CO2 from - 50 to 500 1
with Liquid N2 from - 100 to 500 1
Setting the maximum temperature

This parameter defines the maximum allowable oven temperature setpoint to protect the column
from damage. This limit must be set to the maximum operating temperature recommended by the
producer for that column.
 In order to set the maximum temperature, open the page “Set up”, select “Others” and insert
the value in the text box “Max Oven Temp” (See the chapter “Set up”).
If the temperature value set is higher than the maximum temperature value, the display will show
an alarm message “OVEN:TEMP SET OVER MAX TEMPERATURE”.
This alarm does not allow GC to get the READY status. The condition of error and consequent
message will be eliminated by modifying either the value in the oven program or the value set for
the maximum oven temperature.
In case of the first isotherm, the set value will be accepted in any case, but the oven
temperature will stop at the maximum temperature safety value.
Setting the oven temperature (Rates)

 In order to program the oven temperature, press Menu, select Oven and open the page “Rates”
(fig. 18). Use the numerical keypad to type the initial temperature of the run and press OK, then
insert the length of time, expressed in minutes ( with 0.01 min increment), that you want the oven
to remain at this temperature.
If you want to create a temperature program (up to 25 temperature ramps can be set in a
method), enter a temperature rate, then specify a final temperature and a time, eventually.
The maximum temperature rate for different intervals are shown in the table below. If you enter a
17
Fig. 18 - Oven temp setting
value higher than allowed, both the temperature and rate values will be visualized in red (fig. 18).
In the Alarm page, the message “OVEN RATE TOO HIGH” will be shown.
The maximum value allowed in that interval is automatically suggested when you press on each
box.
Change one of the two values to make the setting acceptable. The alarm will be automatically
recovered.
Fig. 19 -Oven rate too high
18
Maximum rates
Interval (°C) Maximum rate (°C/min)
30 - 70 140
71 - 115 95
116 - 175 70
176 - 300 50
301 - 450 35
451 - 500 30
After setting the temperature program, the total analysis time (expressed in minutes) will be
displayed under the table. The value displayed does not include the cooling time unless it is
included in the program through a negative gradient.
Important
The duration of analysis controls to the performance of all time controlled functions.
In fact, if a PTV injector temperature program or a pressure program has a duration
time higher than the analysis time, it will stop at the end of the analysis.
Furthermore, possible programmed time events, with times higher than the analysis
time will return to initial conditions upon termination of said analysis.
Oven fan (General)

 Open the page “General” (fig. 20) and press the buttons ON or OFF to manually activate
or deactivate the functioning of the oven fan, independently from the oven conditions at the
time. When the oven fan is off, the status OVEN FAN OFF will appear on the Status Bar.
19
Fig. 20 - Oven general page
Pressing the write "OVEN FAN OFF" on the Status bar the "General" page will appear.
Select ON to active the fan.
In case of a rapid oven temperature drop, for example caused by the opening the door, the fan and
the oven heater are automatically turned off and the buzzer beeps 3 times.
The following message will be is shown: “For your safety the Oven fan has been switched off.
Do you want to re-activate it now?”
Close the door and press “Yes” to re-activate it.
Oven Fast Cooling

The oven project allows to reach high speed cooling (Oven fast cooling). This function and the high
speed separations (Fast GC) allow you to maximize the number of analyses.
“Oven fast cooling” is always active. In order to disable this function open the page “Other” in the
window “Set up” (See the chapter headed “Set up”) and press the button "OFF"
Conditioning time (General)

The conditioning step consists of an additional stabilizing time calculated from the moment when
the instrument reaches the ready condition. The READY message will only show at the end of this
step. The duration of this step can vary from 0 to 999 minutes.
 In order to set the conditioning time, open the page “General” (fig. 20) and insert the value
in the corresponding box.
During this step, the message “CONDITIONING” and the elapsed time will be displayed on the
status bar.
Cryogenic system (Cryo)

The cryogenic cooling system allows to reach temperatures below ambient using a cryogenic liquid
as a coolant (-50°C with liquid Carbon Dioxide and -100°C with liquid Nitrogen).
20
The DANI service engineer is suggested to install the device and set the configuration. If you need
to change the configuration see the Chapter “Set up”
 In order to control this device open the page “Cryo” (fig. 21). You’ll find the following functions:
• Cryo: this function enables the oven cryogenic cooling. Press “Yes” to activate it.
• Cryo threshold (°C): this parameter defines the temperature at which the cryogenic
cooling is enabled. Set a temperature close to ambient temperature (+30°C) for regular
operation. Set a higher temperature (+45°C) for a faster cooling of the oven.
• Cryo saving: when this function is ON, the cryogenic cooling and the oven fan are
switched off if a run does not start within a specified time (Cryo saving (min) after the
oven ready. This function generates an alarm: “Cryo time out” . It allows to save
cryogenic coolant in case of automation failure.
• Cryo saving (min): this value ranges from 10 to 120 minutes and represents the time,
calculated from the Ready condition, when the “cryo saving” function occurs.
• Cryo Fault: if the oven temperature doesn’t reach the setpoint within 16 minutes, the
cryogenic cooling will be deactivated. Press ON to activate this function.
Fig. 21 - Oven Cryo page
GCxGC Modulator (General)

 When a Modulator for the GCXGC technique is installed in the Oven and the configuration is
set (see the Chapter “Set up”), the parameter GCxGC Modulator will be displayed in the
page "General" (fig. 23)
If activated, the system takes into consideration the presence of this device and applies an
appropriate temperature control.
It is advisable to press OFF if the device is present, but not working.
21
Temperature indication (Status)
 In order to see the actual oven temperature open the “Status” page (fig. 22). The number
on the right indicates the oven temperature set and that on the left the actual oven temperature
reading as taken by the probe inside the oven.
22
Fig. 23 – Oven Status Fig. 22 – GCxGC modulator
23
Installing the columns
Warning
Warning! The injector must be completely depressurized before doing any maintenance to
the injector
Packed columns
Due to their poor flexibility, the packed columns must be installed into the injector and the detector
at the same time.
The injector end of the column must be empty for at least 60 mm to avoid the syringe
needle entering the stationary phase. This space can be filled with glass wool.
The detector end must be empty for at least 40 mm to avoid the stationary phase damaged by the
detector heating.
Nuts and ferrules
Nuts
To install stainless steel or Teflon packed columns with 6 or 4 mm external diameter use a 1/4G
brass nut. A 17 mm spanner should be used to tighten the nut.
To install glass packed columns it is advisable to use the specific 1/4G brass nut and tighten it
exclusively by end.
The columns with 1/8 inch external diameter requires the use of an adapter to adapt the 1/4G
thread of the injector and detector end to 1/8 inch thread; the 1/8 inch nut of the column is then
installed on this adapter. An aluminum washer assures the tightness between the adapter and the
injector or detector base body.
24
Ferrules
The two-piece brass ferrules are mostly used to install the stainless steel packed columns.
Stainless steel ferrules can also be used but the tightness is more difficult to obtain and there is the
risk to damage the column or the threaded end.
To install the glass columns, the graphite ferrules are recommended.
These ferrules provide excellent tightness even at high temperature (up to 400 °C). Furthermore,
they can be removed without damaging the column as they do not adhere to it permanently.
A brass washer must be put into the nut when a graphite ferrule is used.
The glass and Teflon columns can be installed using Viton O-rings keeping in mind that these ring
cannot be heated at temperature higher than 200 °C and must be changed quite often.
The Viton O-rings are not recommended for analysis at high sensitivity (for example with ECD) as
they can release interfering substances.
An O-ring 104 with a brass washer is used for 6 mm columns.
An O-ring 104 plus 2 O-ring 2015 are needed for 4 mm column; besides, the lower part of a 4 mm
brass ferrule must be put up side down on the bottom of the nut.
Nuts and ferrules used with packed columns are summarized in the table below.
NUTS
Stainless Steel columns
6 mm o.d. 4 mm o.d.
Part. no. 2300 095 01 1

Nut F 1/4G, brass, set of 20 * *
Part. no. 2300 495 001
Nut F 1/8" SW, brass, set of 10
Part. no. 2303 230 040
Adapter F 1/4G-M 1/8SW
Part. no. 2180 095 0081
Washer 6.1x8.0x0.5, Al, set of 20
Part. no. 2300 395 00 1
Nut F 1/4G hand, brass, set of 10
FERRULES
Stainless Steel columns
6 mm o.d. 4 mm o.d.
Part. no. 2306 295 004

Ferrule, BF6, brass, set of 20 *
Part. no. 2306 295 003
Ferrule, BF4, brass, set of 20 *
Part. no. 2306 395 001
Ferrule, BF 1/8", brass, set of 10
25
Packed column installation
Assembling a packed column should be carried out as follow:
• Slide the proper nut onto each end of the column.
• Slide a washer (if required) and a ferrule onto each end of the column. If the ferrule is
conical, this must be slided with the tapered end positioned externally.
• Insert the column into the injector and detector and push the column upwards until it
stops. Partially hand screw the nuts.
• Pull down the column for 1-2 mm and using a spanner, tighten the nut by 1/4 turn
(tighten glass columns only by hand).
• Carry out a leak test on the pneumatic circuit.
Capillary columns
Positioning the column
Capillary columns, because of their flexibility, can be installed between any injector and detector,
independently from their position.
Fused silica capillary columns are usually wrapped on a metal support. The support should be hung
on the hook fitted at the back of the oven. Glass capillary columns or longer and multiple columns
need the appropriate horizontal support (Part. no. 3002 120 000).
When positioning the fused silica capillary column inside the oven, make sure that the terminals
come out of the end of the support without curving excessively or being stretched when connected
to the injector and detector.
Any contact between the column and the wall of the oven must be avoided.
Warning!
Hydrogen (H2) is flammable. Leaks when confined in an enclosed space, may create a fire or
explosion hazard. In any application using hydrogen leak test all connections, lines and valves
before operating.
When using Hydrogen as the carrier gas, be sure that the supply is off until all connection are
made and ensure that the inlet and detector column fittings are either connected to a column or
capped at all time when hydrogen gas is supply to the instrument.
If the Hydrogen flows into the oven can generate an explosion hazard.
26
Preparing the column
Fused silica capillary column

Columns in fused silica have an elevated degree of flexibility, thanks to the external covering in
polyimmide.
No particular preparation process is required.
It is, in any case, indispensable that the edges of the column are uniform and free of any particles
originating from the column itself, coming from the stationary phase or ferrule residue.
It is advisable, therefore, to cut one centimeter of column from both ends before inserting the
column, but after having assembled the nuts and ferrules.
In order to do this, first cut into the column with a glass cutter or file at the point in which it should
be cut, then snap off by hand.
Important
While carrying out the aforesaid operation it is advisable to wear protective goggles and
gloves to protect hands and eyes from possible injury caused by fused silica particles.
These precautions should be respected even more rigorously when handling wide bore
columns which are more rigid.
Glass capillary columns

Glass capillary columns are extremely fragile, therefore, installation requires particular care. For a correct
installation, it is fundamental that the column extremities are perfectly straight.
Nuts and ferrules
Nuts
To install both capillary and wide-bore capillary columns SS nut F 4M (1). A 7 mm spanner
should be used to tighten the nut.
Ferrules
Two types of ferrules are available for installing capillary columns: graphite ferrules and
vespel-graphite ferrules.
27
Graphite ferrules have a high degree of seal, are long lasting and can be used at high
temperatures (up to 450°C); they are usually recommended for glass capillary columns.
Since they do not adhere permanently to glass, they can be removed without the risk of damage to
the column. They must always be used together with a brass washer (2).
They are available in one size only since they can be adapted to different capillary column
diameters.
Vespel-graphite ferrules are specific for capillary columns. They can be used with temperature of
up to 350°C and are usually re-usable. These ferrules are subject to leakages or cracks if tightened
excessively while cold. They must always be used together with a brass washer (2).
These ferrules are available with through holes of different diameters, adapt for different external
column diameters.
The table below shows the blockages and ferrules to be used according to the type of capillary
column.
NUTS
Fused silica columns Glass

Columns
< 0.< 25 mm i.d. any
0.25 mm i.d. 0.32 mm i.d. 0.56 mm i.d.
diameter
Part. no. 2300 590 004

Nut F 4M, SS, + washer * * * * *
Part. no. 2180 014 002
Washer 4M, brass, set of 10 * * * * *
FERRULES
Fused silica columns Glass

columns
< 0.< 25 mm i.d. any
0.25 mm i.d. 0.32 mm i.d. 0.56 mm i.d.
diameter
Part. no. 2180 095 020

Ferrule 3x2x1, graphite, set of 50 * * * * *
NUTS
Part. no. 2306 095 003

Ferrule 0.76 mm, VGR, set of 10 *
Part. no. 2306 095 002
Ferrule 0.46 mm, VGR, set of 10 *
Part. no. 2306 095 001
Ferrule 0.36 mm, VGR, set of 10 * *
28
Assembling the glass liner
Split/splitless injector
The split/splitless injector must be used with a specific glass liner (Part.no. 9291.100 003).
It consists of a tube in borosilicate glass of correct dimensions and containing silanized glass wool,
a graphite ferrule in a steel cylinder and a steel friction washer.
The liners supplied by DANI are washed and conditioned at high temperatures.
If a silanized liner is needed, proceed to the cold silanization as explained in the section headed
“Procedure for Silanization of precolumns” in the chapter “Introduction System –

Injector Maintenance”
The assembling of the liner (fig. 24) is not necessary when using a new instrument, since it is
already inserted in the injector.
In all other cases, assembly of the liner should be carried out as follows:
Caution!
The temperature of Oven, Injector and/or detector might be high enough to cause burns
Fig. 24 - Assembling the split/splitless liner
• Before removing the septum holder (1) which contains the introduction septum (2),
disable the flow control (see Introduction systems) and wait until the pressure reaches 0
bar.
29
• Remove the internal steel ring (3), using the special spanner, which is supplied, on the
side which has two dots.
• With the aid of a pair of pliers, take out the spring (4) from the injector and the
precolumn, if there is one (7).
• Taking care as much as possible to avoid contamination, insert the new precolumn,
complete with ferrule (6) and washer (5), into the injector.
• Using the threaded end of the special spanner, tighten the graphite ferrule on the
precolumn body.The procedure is to screw the spanner onto the threaded part inside the
injector. Give the spanner a quarter turn at a time until a certained resistance is felt.This
operation is only necessary when a new precolumn is being fitted.
• Return the spring into the body of injector.
• Reposition and screw the internal ring, with the special spanner, until it is lined up with
the external edge of the injector.
• Refit the septum holder complete with injection septum.
Warning
Avoid tightening the septum holder more than necessary. This could cause difficulties
when introducing the needle of the syringe. This can also create septum fragments that
can consequently contaminate the liner and generate instability in the flow control.
PTV injector
A specific liner must be used with the PTV injector.
It differs from the liner used with the split/splitless injector in form and dimension.
It is a borosilicate glass tube in an adequate size which contains silanized glass wool, a graphite
ferrule in a steel cylinder and a steel friction washer.
Special liners for the PTV injector which contain a sorbent material (e.g. Tenax or Carbosieve) are
also available for special applications.
Liners supplied by DANI are washed and conditioned at high temperatures.
If a silanized liner is needed, proceed to the cold silanization as explained in the section headed “
Procedure for Silanization of precolumns”, in the chapter “Introduction System”.
Caution!
The temperature of Oven, Injector and/or detector might be high enough to cause burns
30
The assembly of the liner is not necessary when using a new instrument since it is already
inserted in the injector.
In other cases, assembly of the liner should be carried out as follows (fig. 25):
• Remove the septum holder (1) which contains the introduction septum (2).
• Remove the internal steel ring (3), using the special spanner, which is supplied, on the
side which has two dots.
• With the aid of a pair of pliers, take out the spring (4) from inside the injector and the
precolumn, if there is one (7).
• Taking care as much as possible to avoid contamination insert the new precolumn,
complete with ferrule (6) and washer (5), into the injector.
• Using the threaded end of the special spanner, tighten the graphite ferrule on the
precolumn body.The procedure is to screw the spanner onto the threaded part inside the
injector. Give the spanner a quarter turn at a time until a certained resistance is felt.
This operation is only necessary when a new precolumn is being fitted.
• Return the spring into the body of injector.
• Reposition and screw the internal ring, with the special spanner, until it is lined up with
the external edge of the injector.
• Refit the septum holder complete with injection septum.
Fig. 25 - Assembling of the PTV injector liner
31
Warning
Avoid tightening the septum holder more than necessary. This could cause difficulties
when introducing the needle of the syringe. This can also create septum fragments that
can consequently contaminate the liner and generate instability in the flow control.
Installation of capillary column

The installation procedure for the column is identical for both the split/splitless injector and the
PTV injector.
Identify the correct nut and ferrules for the column to be installed (see section headed Nuts and
Ferrules in this chapter) and carry on the column installation as follows (fig. 26):
Fig. 26 - Nut and ferrule installation
Slide a nut (1) onto each end of the column, with the threaded part positioned externally, followed
by a brass washer (2) and a ferrule (3).
If a vespel-graphite ferrule is used, this must be slide with the tapered end positioned externally.
The drawing here below illustrates the correct assembly sequence.
After assembling the seals, 1 cm of column should be cut from each end (see the section
Preparing the column in this chapter).
Installation of the column at the injector
32
Fig. 27 - Positioning the nut at the injector
• Check that the glass precolumn and other parts have been correctly inserted inside the
injector (refer to section Assembly of precolumn in this chapter).
• Attach the column cage to the two hooks on the back wall of the gas chromatograph
oven.
• Free the end of the column which is positioned towards the injector in order to avoid any
tension.
• Move the nut along the column until the distance between the end of the column and the
base of the nut measures 23-25 mm, then mark the point with an indelible marker or
liquid corrector (fig. 27).
• Insert the column into the injector and partially hand screw the nut.
• Push the column upwards until the marked point is in line with the base of the nut.
The column will now be 1-2 mm inside the precolum.
• Using the pitch 7 spanner supplied, the nut should be tightened by 1/4 turn.
Avoid over tightening the nut since it could break the column
33
Installation of the column in the Flame Ionization Detector
Fig. 28 - Positioning the column nut for FID
• Free the end of the column which is positioned towards the detector in order to avoid any
tension.
base of the nut measures 65-66 mm, then mark the point with an indelible marker or
liquid corrector (fig. 28).This operation is not necessary if a column with external
diameter higher than 0.25 mm must be installed as it does not pass through the hole of
the jet.
• Insert the column into the detector and partially hand screw the nut.
• Push the column upwards until the marked point is in line with the base of the nut. The
end of the column will now be 1-2 mm below the upper tip of the nozzle.
In the case of a column with the external diameter higher than 0.25 mm, it is possible to
push the column upwards until it stops, tighten the nut by hand and pull the column down
for 1-2 mm.
• Using the pitch 7 spanner supplied, the nut should be tightened by a 1/4 turn. Avoid
over tightening the nut since it could break the column.
Installation of the column in the Electron Capture Detector

tension.
base of the nut measures 55 mm, then mark the point with an indelible marker or liquid
corrector.
• Using the pitch 7 spanner supplied, the nut should be tightened by a 1/4 turn.
Avoid over tightening the nut since it could break the column.
34
Installation of the column in the Photoionization Detector
tension.
base of the nut measures 10 cm, then mark the point with an indelible marker or liquid
corrector.
Installation of the column in the Nitrogen - Phosphorus Detector

tension.
base of the nut measures 10.3 - 10.4 cm, then mark the point with an indelible marker or
liquid corrector.
This operation is not necessary if a column with external diameter higher than 0.25 mm
must be installed as it does not pass through the hole of the jet.
• Push the column upwards until the marked point is in line with the base of the nut. The
end of the column will now be 1-2 mm below the upper tip of the nozzle.
In the case of a column with the external diameter higher than 0.25 mm, it is possible to
push the column upwards until it stops, tighten the nut by hand and pull the column down
for 1-2 mm.
Installation of the column in the Thermal Conductivity Detector

tension.
base of the nut measures about 40 mm, then mark the point with an indelible marker or
liquid corrector.
• Proceed in the same way to install the column in both the detector channels.
35
Installation of the column in the Flame Photometric Detector
tension.
base of the nut measures about 14.3 - 14.5 cm, then mark the point with an indelible
marker or liquid corrector.
The column will stand out of the nozzle for about 0.8 - 1.0 cm.
• Proceed in the same way to install the column in both the detector channels.
Leak testing the pneumatic circuit

See Chapter "Diagnostics" paragraph "Leak test”
Conditioning the columns

The columns must be conditioned before use.
DANI columns have been pre-conditioned, however, to get excellent performances and to remove
any possible contaminant coming from the liner septum and column handling, we recommend
conditioning again the column. The procedure is even more essential for used columns since they
may also contain residual composites from previous introductions.
The conditioning procedure should be carried out as follows:
• Assemble the column in the chromatograph oven connecting the terminal to the injector
end only and leaving the other end free.
If the column is connected at both ends, the alternative is to remove the detector head
from the base body (except in the case of a ECD detector).
• Switch on the carrier gas and set a flow which is suitable for the type of column.
• Set a temperature program which starts from a relatively low temperature (40 - 60 °C)
and reaches a final temperature 20°C above the operating temperature without
exceeding the maximum allowed for the column, using a gradient of 2-4°C/min.
• Condition the column for 4-6 hours, setting a suitable number of analytical cycles. (When
the operating temperature is the maximum allowed, a longer conditioning time may be
necessary).
36
Introduction systems
Packed column injector
Description
The packed column injector DANI IN 86/06 is capable to operate with stainless steel columns
with 6 mm, 4 mm or 1/8 inch outer diameter and glass column with 6 mm outer diameter. It
can be used also with wide-bore columns by means of a special adapter.
The injector (fig. 29) consists of a cylindrical stainless steel body (1) on which a carrier gas line is
inserted (2).
The body is welded to a support (3) which is fixed to the gas chromatograph by two screws.
The injector is closed by an external ring (4) which holds the introduction septum (5). Inside, a steel
cylinder (6) leads the syringe needle directly into the column.
The body is directly heated by an aluminum block (7) which contains the heating resistance and
the temperature probe.
Both glass and stainless steel packed columns are inserted directly into the injector body.
Therefore, the necessity of precolumn or liner is eliminated, dead volume is minimized and the
compounds are directly injected into the column.
For this reason, the column end at the injector side must be free of stationary phase for at least a 6
cm length and filled with glass wool only.
As the carrier gas flow rates normally used with packed columns are high (about 30 ml/min) and
the injector volume is of a few hundred of microliters, the transfer of the sample is fast enough.
Fig. 29 - Packed column injector
37
Pneumatic circuit
The pneumatic circuit of the packed column injector, illustrated in figure 30, consists of the carrier
gas line only.
An electronic control module is installed on the carrier gas line to control the flow rate or the
pressure.
When packed or undefined columns are used, the electronic control module is automatically
configured as a flow regulator.
The flow rate is controlled by the Total Flow Regulator “TFR” while an Injector Pressure Sensor
“IPS” measures the actual pressure at the injector.
Fig. 30 - Packed column injector pneumatic circuit
The flow rate in the packed column varies considerably with the temperature: if the pressure at the
head of the column is constant, the flow rate decreases when the temperature increases.
The flow regulator acts by increasing the pressure at the head of the column when the
temperature increases, thus maintaining the desired flow rate .
In this way, analyses with programmed temperature at constant or programmed flow rate can be
performed .
When wide-bore capillary columns of defined dimensions are used, the electronic control module is
automatically configured as a pressure regulator (fig. 31).
The Injector Pressure Regulator “IPR”, connected at the Injector Pressure Sensor “IPS”, maintains
the needed pressure at the head of the column, to guarantee the desired flow rate.
38
Fig. 31 - Pneumatic circuit with wide-bore column
Adapter for wide-bore capillary column

The packed column injector may be used with fused silica wide-bore columns (> 0.50 mm i.d.)
using the special adapter supplied with the instrument (Part.no. 0305.047 003). In this
configuration, the carrier gas flow rate must be high enough to guarantee a fast transfer of the
sample into the column.
The adapter for wide-bore (fig. 32) columns.must be inserted from the bottom of the injector
body and locked with a nut (2) and a brass ferrule (3).
A glass liner (4) filled with glass wool is inserted inside the body from the upper part after
unscrewing the external screw and taking off the steel cylinder.
Fig. 32 - Adapter for wide-bore columns
To install the wide-bore capillary columns on the adapter, follow the same procedure described for
the capillary injectors (refer to Capillary columns in the chapter Installing the columns).
39
Injector temperature (Temp)
The temperature of the packed injector is normally set at about 50 °C higher than the boiling point
of the solvent used in the sample or equal to the elution temperature of the heavier compound.
Too high temperature can increase the risk of decomposition of the sample or discrimination
effect.
 To set the injector parameters, press the corresponding shortcut key or select Menu,
Injector then A, B or C.
To enter the temperature value, open the page “Temp” and press ON to enable the temperature
control. Pressing on the box, the numeric keypad will appear. Digit the number and press OK to
confirm the setpoint (fig. 33).
Fig. 33 - Injector temperature
Carrier Gas Control (press/flow and column)

When a packed/undefined column is selected, the carrier gas of a packed injector can be controlled
in two different modes:
• Constant flow: the column flow is constant during the analysis. The pressure at the
head of the column will increase with the oven temperature to maintain a constant flow.
• Programmed flow rate: in programmed flow mode the column flow rate can be set to
change during the analysis. You can enter up to 25 flow ramps.
When a capillary column is configured, constant pressure and programmed pressure
modes are also available.
• Constant pressure: in this mode the pressure is constant during the analysis. The
flow will change with the oven temperature.
40
• Programmed pressure: in this mode the inlet pressure can be set to change
during the analysis. You can enter up to 25 pressure ramps
 Open the page “Column”, select the carrier gas and the column type between
packed/undefined or capillary.
If you select an unpacked column you have to set the "max pressure" value. The “max pressure”
is the highest pressure value that the system is expected to reach during the temperature
program. It is used to define the pressure range for a certain column and optimize the flow
regulation in that range: the longer the column or the smaller diameter or the higher particle
mesh, the higher the pressure range. The maximum acceptable value is 6 bar.
To establish this value, set it first at 6 bar and then run your temperature program. Take note of
the maximum actual pressure value and set it for all the subsequent analyses. Please,
remember that the pressure at the GC inlet must be ca. 2 bar higher than the “max pressure”
setpoint. (fig.34)
Fig. 34 - Column type Fig. 35 - Column dimension
Fig. 36 - Press/Flow control
If you select a capillary column, you have to specify also the dimensions (fig. 35).
Open the page “Press/Flow to select the control mode and the pressure or flow rate values
(fig.36).
41
Split/splitless injector
Description
The split/splitless injector can be used with all types of narrow bore and wide-bore capillary columns.
The injector (fig. 37) consists of a cylindrical steel body (1) on which a carrier gas line inlet (2) and the
split (3) (SPLIT) and septum wash (PURGE) (4) gas lines outlet are inserted. The body is welded to a
support (5) which is fixed to the gas chromatograph by two screws. A glass liner (6) is inserted into the
body: a reinforced graphite seal (7) with a steel washer (8) will guarantee isolation between the upper
and lower parts of the injector body. The upper part contains a spring (9) and an internal ring (10)
through which the carrier gas flows.
The injector is closed by an external ring (11) which holds the introduction septum (12).
Fig. 37 - Split/Splitless injector
42
The injector is heated directly by an aluminum block (13) which contains the heating resistance
and the temperature probe. To guarantee the insulation of the injector, an insulation cover (16)
containing glass wool (14) and a washer in SILIT (15), covers the part of the body inside the Oven.
The cover is fixed by a nut (17).
Pneumatic circuit
The pneumatic circuit of the split/splitless injector consists of three gas lines: the carrier gas inlet
line, the split gas line and the purge line.
An input electronic control module is installed on the carrier gas line of injector. The purge and split
lines are connected at the output electronic control module. A molecular sieve filter “FLT” protects
the split line from contamination.
The input and output electronic control modules are automatically configured depending on the
injection technique utilized.
Fig. 38 - Pneumatic circuit in split mode
When the injector is in “split mode”, the input electronic control module works as a flow regulator
(fig. 38).
A total flow rate consisting of the sum of column, split and purge flow rates os regulated by the
Total flow regulator (TFR).
The Injector BackPressure Regulator (IBPR), connected to the Injector Pressure Sensor (IPS) ,
maintains the needed pressure at the head of the column to guarantee the desired flow rate into
the column.
The Purge flow rate is controlled by the Purge Flow Regulator (PFR) while The Split flow rate is the
difference between Total flow and Purge flow.
When the injector is in “splitless mode”, the input electronic control module operates as a pressure
regulator (fig. 39).
The Injector Pressure Regulator (IPR), connected to the Injector Pressure Sensor (IPS) , maintains
the needed pressure at the head of the column to guarantee the desired flow rate. The Purge flow
rate is controlled by the Purge Flow Regulator (PFR).
Split flow rate is blocked as the Injector BackPressure Regulator is closed.
43
Fig. 39 - Pneumatic circuit in splitless mode
Injector temperature
In the split/splitless injector, the liquid sample must be volatilized as quickly as possible.
In order to obtain this result, the injector must be 20-30 °C above the maximum oven temperature
set for the analysis.
When the splitless technique is used (see Introduction Techniques, in this chapter), the
permanence time of the sample in the injector is higher than that of the split technique.
It is, therefore, advisable to set the injector temperature at a slightly lower value.
The ideal temperature is the minimum temperature at which complete vaporization of the sample
is obtained (therefore, the maximum area of peaks) without giving signs of thermal degradation of
the compounds.
 To set the injector parameters, press the corresponding shortcut key or select Menu, Injector
then A, B or C.
Fig. 40 - Injector temperature
To enter the temperature value, open the page “Temp” and press “On” to active the temperature
control. If you press on the box a numeric keypad will appear. Digit the number and press OK to
confirm the setpoint. (fig. 40 ).
44
Carrier Gas Control (Press/flow and Column)

The carrier gas of a split/splitless injector can be controlled in five different modes:
head of the column will automatically increase with the oven temperature to maintain a
constant flow.
flow will decrease with the oven temperature.
during the analysis. You can enter up to 25 pressure ramps.
• Linear velocity: in this case Master GC maintains the carrier gas linear velocity constant
during the column temperature program.
 Open the page “Press/Flow” (fig. 42) to select the control mode and insert flow, pressure
or linear velocity parameters.
Fig. 42 - Carrier gas control Fig. 41 - Column Specifications
The carrier gas control takes into consideration the column specifications. To allow the GC to work
correctly in the selected mode, open the page “Column” and enter the carrier gas type and column
dimensions (fig.41 ).
45
Warning!
before operating.
Injector depressurization: Before starting any maintenance to the injector it is necessary to

depressurize the injector to avoid that the glass wool inside the liner moves.
When the Press/Flow Control is OFF the injector pressurization starts automatically. The split valve
is opened to drop the pressure slowly.
During this procedure the following pop-up will be displayed: "Please, wait for the depressurization
to end before doing any maintenance to the injector" (fig. 43).
Fig. 43 - Injector depressurization
Injection techniques
The split/splitless injector can operate according to three injection techniques:
• the split injection, for analyzing main components

• the splitless injection, for analyzing trace components
• the pulsed injection
Split injection
Introduction of a sample with the split technique consists on injecting the sample into a hot
injector.
46
The generated vapors are divided into two different parts: one part is carried into the column by
the carrier gas and the other is discharged outside through the split line.
The ratio between the quantity of gas entering the column and the quantity discharged is
proportional to the ratio of gas flowing into the column and the flow of gas exiting from the split.
The split ratio is normally referred to the unit of the carrier gas flow rate, that is:
carrier flow rate split flow rate

split ratio = :
carrier flow rate carrier flow rate
where volumetric flow capacities are in ml/min.
For example, if the column flow rate is 2 ml/min and the split flow rate is 100 ml/min, the split ratio
is:
2 ml / min 100 ml / min

split ratio = : = 1 : 50
47
 To operate in split mode open the page “Split” and select “Split” at the item “Mode”
“Split Flow” and “Split Ratio” values are correlated. If you insert the split flow value, the split ratio is
automatically calculated and vice versa. The split ratio value is the ratio between the split flow and
the column flow. (fig. 44 ).
Fig. 44 - Split mode
Manual injection (Double Start)
When the autosampler is not configured or the autosampler sequence is OFF, the GC is in
Manual Injection Mode. In this case when all parameters are ready, the GC status will be "Stand
by" and on the Start button the inscription will be "prep".
Pressing the start button the first time before the injection, the GC status will become "Ready" and
the injection can be performed within 25 seconds from the Ready status.
After the introduction press "start" the second time to begin the measurement.
In case of automatic injection, the passage from the “Stand-by” to the “Ready” status will be
automatically performed.
Splitless introduction
When using the splitless technique, the sample evaporates completely in the hot injector. When
introduction is carried out the split gas line is closed, and all the sample goes into the column.
At a certain time after introduction, the split gas line is opened. In this way, the excess of solvent is
discharged outside. The solvent peak, which otherwise would be so extended as to cover a large
portion of the initial part of the chromatogram, is significantly reduced in width.
The opening time of the split valve depends on the components, the solvent, the volume of
sample introduced and the flow rate of the carrier gas.
It is usually within a range between 20 seconds and 2 minutes.
The ideal opening time is one which gives the major response for the compounds of interest.
48
In splitless injection, the absolute split flow rate is not important: set a split flow rate high enough
to purge the injector (40-50 ml/min is a suitable flow rate).
Transfer of the sample into the column is slower when using the splitless injection method
compared to the split method.
Therefore, in order to reduce the subsequent widening of the peaks, the initial column
temperature should be set at a relatively low value (20-30 °C below the solvent boiling point):
under these conditions the solvent re-condenses and the components refocus in a narrow band
at the column head (Solvent effect) to be subsequently eluited in a temperature program.
When the splitless introduction technique is used, it is important to verify the purity of the solvent
used to dilute the sample, since any impurities will re-concentrate at the column head and can
interfere with the peaks under investigation.
It is advisable to carry out the analysis of a blank in order to verify the purity of the solvent.
The technique is more complex but, as the opening and closing action of the valves is
automatically performed, it is perfectly repeatable.
 To operate in splitless mode open the page “Split” and select “Splitless ”at the item “Mode”.
Set the split flow value used to purge the injector into the box “Split purge” and the time,
calculated from the start of the analysis, at which the split valve will be opened into the box “Split
ON” (fig.45 ).
Fig. 45 - Splitless mode
In the splitless mode, when all setpoints are reached, the split line remains open, the inscription
“Prep” will appear in the “Start” shortcut key and “Stand by” will be displayed in the Status bar.
To perform a manual injection, press “Prep”: the split valve will close and in the Status Bar the
inscription “Ready” will appear.
Insert the syringe into the injector, inject the sample and withdraw the syringe rapidly. Then press
“Start”.
49
Pulsed injection
When using the pulsed technique, a higher inlet pressure is activated, during the injection step,
for a preset time.
Increasing the pressure during the injection reduces the expansion volume, temporally increases
the column flow rate thus improving the transfer of the analytes into the column. This effect is
especially useful in splitless injections where the column flow rate during the sample transfer is
reduced.
 To operate in this mode, it is necessary to set the pressure value at the injection time and
the duration of the pulsed pressure.
Open the page “Press/Flow” and press the button “Pulsed inj”. Insert into the boxes the “Pulsed
pressure” value and the “time”, then press ON to activate this mode. (fig. 46).
In case of splitless injection, it is advisable to set the same “time” as in the “Split On”
parameter.
In the pulsed injection mode, when all setpoints are reached, the carrier gas pressure remains at
the value set in the method, the inscription “Prep” will appear in the “Start” shortcut key and
“Stand by” will be displayed in the Status bar.
To perform a manual injection, press “Prep”. The injector pressure increases up to the pulsed
pressure set point and in the Status Bar the inscription “Ready” will appear.
Insert the syringe into the injector and pay attention to the plunger of the syringe, in fact the
high pressure could blow away the plunger if not correctly kept. Inject the sample and withdraw
the syringe rapidly. Then press “Start”. The pressure at the injector remains at the higher value
temporary during the pulsed pressure period.
Fig. 46 – Pulsed Injection Fig. 47 – Septum Purge
50
Purge flow rate

In a chromatographic system, especially with capillary columns, the introduction septum is an
evident source of contamination. For this reason the split/splitless injector is equipped with a purge
line which provides a constant flow that purges the introduction septum in the internal area of the
injector.
Usually, a 3-6 ml/min purge flow rate is a suitable value.
The purge line is fed by the carrier gas itself.
 To set the flow rate of gas flowing into the purge open the page “Split” and press the
button “Purge”. Insert the value in the corresponding box. (fig. 47 ).
Gas saving
The “Gas saving” reduces the carrier gas flow rate from the split vent after the sample has been
transferred into the column until the next injection, thus saving amounts of gases.
 To set the value open the page “Split” and press the button “Gas saving” (fig 48). Press ON
to turn on the gas saving flow and insert in the box “Flow” the setpoint value. The split flow rate
will be reduced immediately, the “Stand by” status will be showed on the toolbar and “Prep” will
appear on the Start shortcut key.
Fig. 48 - Gas saving
In the box “Time” enter the time during the run when the split flow rate is reduced (fig. 48). In
case of split injection, set a time after the injection time. In case of splitless and/or pulsed
injection, set a time after the splitless or pulsed time.
Pressing “Prep ” will restore the initial split flow rate and “Ready” will be showed on the status bar .
51
Introducing the sample
In order to have quantitative and repeatable data with a split/splitless injector, a correct sample
introduction technique must be used to limit the well known discrimination phenomenon. This is
particularly important when the sample contains components in a wide range of concentrations
and which differ in volatility and polarity.
It has been demonstrated that the discrimination phenomenon in the sample is mainly at the
syringe needle level.
When the syringe needle is introduced in the septum, it accumulates heat from the injector, this
resulting in the partial evaporation of the more volatile substances inside the needle itself.
When the syringe plunger is pushed, the solvent and the more volatile substances evaporate more
rapidly than substances with a higher boiling point, subsequently, these tend to remain into the
internal walls of the needle.
Therefore, when the needle is removed from the injector, a fraction of the non volatile components
is also removed.
The result is a discrimination phenomenon caused by the volatility level of each component.
This discrimination effect can be minimized by optimizing the introduction technique regarding
both the operative parameters and correct use of the syringe.In consideration of this point, it
should be noted that the condition of the syringe being used is fundamental to obtain good
results.Syringes which have imperfections such as deformations or leaks should be discarded.
Use of an automatic sampler will noticeably improve repeatability as opposed to manual

introduction: each step of introduction is identical for each injection.
Different methods of using the syringe have been documented (full needle, cold empty needle, hot
empty needle, solvent plug, air plug).
The Hot needle technique results, for many research workers, as being the technique which
provides the best results.
The Hot needle introduction technique is as follows:
• Take the sample, in direct contact with the plunger, and measure the required quantity.
• Aspirate the all sample into the cylinder of the syringe.
• Introduce the needle into the injector.
• Wait a few seconds (3-5 sec.) until the needle reaches the temperature of the injector.
• Introduce the sample by pushing the plunger as quickly as possible and extract the
syringe within one second.
This method guarantees a minimum of discrimination, even if total elimination is not possible,
more especially with compounds which have very different volatility levels.
In the case of thermolabile compounds, which can degrade in contact with the hot metal surface of
the needle, an alternative is to use the solvent plug technique.
The procedure is the following:

52
• Clean the syringe by filling and emptying it several times using the solvent, then eliminate
any excess. The needle volume will be filled with solvent.
• Aspirate a significant volume of air.
• Aspirate a more than adequate quantity of sample.
• Regulate the plunger on the level of the required sample volume by measuring the
difference with the air volume then eliminate any excess.
• Aspirate the total volume of liquid (solvent + air + sample) into the cylinder of the
syringe.
• Introduce the syringe into the injector.
• Push the plunger quickly then extract the syringe from the injector.
53
PTV Injector (Programmed Temperature Vaporizer)

Description
The PTV injector (fig. 49) is equivalent to a split/splitless injector which does not have a constant,
but a programmed temperature.
In this case the sample is introduced into the injector at a low temperature. When the syringe is
extracted, the injector is then brought rapidly to a high temperature.
The temperature can be programmed in a linear manner, that means a temperature gradient
can be set.
The injector is composed of a steel cylinder body (1) where the carrier gas line (2) enters and the
split lines (3) as well as the septum purge gas line (4) exits.
The body is welded to a support (5) which is fixed to the gas chromatograph by two screws.
A glass precolumn (6) is inserted into the injector body: a reinforced graphite seal (7) with a steel
washer (8) will guarantee insulation between the upper and lower parts of the injector body.
Fig. 49 - PTV injector
The upper part contains a spring (9) and an internal ring (10) through which the carrier gas flows.
The injector is closed by an external ring (11) which holds the introduction septum (12).
The injector is heated by a heating resistance (13) which is wrapped around the cylinder body
itself.
54
The temperature probe (14) is positioned near the body.
Cooling is obtained by immission of ambient air through a small fan (15) located on the top of the
instrument.
Pneumatic circuit
The pneumatic circuit of the PTV injector is identical to the split/splitless circuit. Therefore, refer to
the description reported in the paragraph Pneumatic circuit of the split/splitless injector in this
chapter.
Injector temperature (Temp)

In the PTV injector, the liquid sample is introduced maintaining the injector at a temperature lower
than the boiling point of the solvent.
After introduction, the injector is rapidly heated at a temperature high enough to vaporize all the
components of the sample.
 To set the injector parameters, press the corresponding shortcut key or select Menu,
Injector then A, B or C. Press ON to enable the temperature control and use the numeric
keypad to insert the temperature, time and rate values. Press OK to confirm the setpoint (fig.
50).
Fig. 50 - PTV temperature
Cryogenic system (Cryo)
The cryogenic system allows to reach a very low oven temperature utilizing a liquid as a coolant
(-50°C with liquid carbon dioxide and -100°C with liquid nitrogen).
A DANI service engineer is suggested to install the device and set the configuration. If you need to
change the configuration see "Inj" in the chapter headed "Set up"
 In order to control this device open the page "Temp". You'll find the following functions:
• Cryo: This function enables the system. Press "Yes" to active it.
55
• Activation Temp (°C):This parameter defines the temperature at which the cryogenic
system occurs.
56
Carrier Gas Control (Press/Flow and Column)

The carrier gas of a PTV injector can be controlled in five different modes:
column head will automatically increase with the oven temperature to maintain a
constant flow.
flow will decrease with the oven temperature.
during the analysis. You can enter up to 25 pressure ramps.
• Linear velocity: in this case Master GC maintains the carrier gas linear velocity constant
during the column temperature program.
 Open the page “Press/Flow” (fig. 51) to select the control mode and insert flow, pressure or
linear velocity values.
Fig. 52 – Carrier Gas Control Fig. 51 – Column dimensions
The carrier gas control takes into consideration the column specifications. To allow the GC to work
correctly in the selected mode, open the page “Column” and enter the carrier gas type and column
dimensions (fig. 52).
57
Warning!
before operating.
Injector depressurization: Before starting any maintenance to the injector it is necessary to

depressurize the injector to avoid the glass wool inside the liner moves.
When the Press/Flow Control is OFF the injector pressurization starts automatically. The split valve
is opened to drop the pressure slowly. During this procedure the following pop-up will be
displayed: "Please, wait for the depressurization to end before doing any maintenance to the
injector" (fig. 53).
Fig. 53 -Injector depressurization
Introduction techniques (Split)

than the boiling point of the solvent.
After introduction, the injector is rapidly heated at a temperature high enough to vaporize all the
components of the sample.
The injection may be performed according to four different modes (fig. 54):
58
• split injection
• splitless injection
• solvent split injection
• pulsed injection
Fig. 54 - PTV Injection mode
Split injection
In the split technique, the sample vapours are divided into two parts: the minimum part enters the
column, the remaining part is eliminated to the outlet through the split vent.
than the boiling point of the most volatile component.
The ratio between the quantity of gas entering the column and the quantity discharged is
proportional to the ratio of gas flowing into the column and the flow of gas exiting from the split.
The split ratio is normally referred to the unit of the carrier gas flow rate, that is:
carrier flow rate split flow rate

split ratio = :
carrier flow rate carrier flow rate
where volumetric flow capacities are in ml/min.
For example, if the column flow rate is 2 ml/min and the split flow rate is 100 ml/min, the split ratio
is:

split ratio = : = 1 : 50
As the syringe needle is withdrawn, the injector is rapidly heated. The split line is constantly open
(fig. 55).
The main advantages of the split injection performed with the PTV injector, respect to the
introduction with the split/splitless injector, are the followings:
• The selective evaporation of the sample inside the syringe needle is eliminated. This
phenomenon is considered one of the main sources of discrimination as high boiling
59
substances vaporize less than the more volatile ones and then remain partially in the
needle.
• Besides, the degradation of thermolabile compounds on the hot surface of the syringe
needle is avoided.
60
Fig. 55 - PTV split mode: split and temperature profile
• cold introduction permits precise quantification of the sample amount introduced as well
as an accurate and linear splitting with a minimum discrimination effect. Therefore, it is
the ideal technique for introduction of small quantities in an extremely repeatable and
accurate manner.
 To operate in split mode open the page “split” and and at the voice “Mode” select “Split”
“Split Flow” and “Split Ratio” values are correlated. If you insert the split flow value, the split ratio is
automatically calculated and vice versa. The split ratio value is the ratio between the split flow and
the column flow (fig. 56).
Fig. 56 - Split injection
61
Manual injection (Double Start):
When the autosampler is not configured or the autosampler sequence is OFF, the GC is in
Manual Injection Mode. In this case when all parameters are ready, the GC status will be "Stand
by" and on the Start button the inscription will be "prep".
Pressing the start button the first time before the injection, the GC status will become "Ready" and
the injection can be performed within 25 seconds from the Ready status.
After the introduction press "start" the second time to begin the measurement.
Splitless injection
In splitless injection mode, the liquid sample is introduced into the evaporator with the split line
closed.
After the major quantity of sample has been transferred to the column, the split line is opened and
the excess solvent eliminated.
Therefore, the splitless technique is suitable for highly diluted solution samples.
Unlike in the split/splitless injector, splitless introduction in the PTV is carried out at a low
temperature.
The initial injector temperature must be lower that the solvent boiling point temperature.
A few seconds (2-3 secs) after introduction, the injector is rapidly heated to a temperature at
which the sample evaporates completely. When enough time has elapsed for the transfer of the
sample to the column (30-90 seconds), the oven temperature program begins and the split line
opens: in this way, any residual solvent is eliminated.
Fig. 57 - Splitless injection: Split and temperature profile
With splitless introduction, the transfer of the sample from the injector to the column is slower
than with split introduction.
In order to reduce the widening of the peaks, the initial column temperature must be set at a
relatively low value (20-25 °C lower than the solvent boiling point): in this way the solvent will
62
re-condense and the components will re-focalize on a narrow band at the column head (Solvent
effect), to be consequently eluted in a temperature programme.
 To operate in split mode open the page “split” and and at the item “Mode” select “Splitless.”
Into the box “Split purge” you can set the split flow value and into “Split ON” the time during the
run at which the “Split purge” valve will be opened (fig. 58).
Fig. 58 - Splitless injection
In the splitless mode, when all setpoints are reached, the split line remains open, the inscription
“Prep” will appear in the “Start” shortcut key and “Stand by” will be displayed in the Status bar.
To perform a manual injection, press “Prep”: the split valve will close and in the Status Bar the
inscription “Ready” will appear.
Insert the syringe into the injector, inject the sample and withdraw the syringe rapidly. Then press
“Start”.
Solvent split injection

With this technique, the sample is introduced in the injector maintained at a low temperature with
the split valve open. After most of solvent has been eliminated, the split line closes and the
temperature rapidly increases (fig. 59).
In this way, these effects are obtained:
• the elimination of most of the solvent and therefore the possibility to detect also early
eluting peaks.
• the possibility to increase the injection volume and to perform repeated injections to
concentrate a very diluted sample.
The only drawback of this technique is the possibility to analyze only compounds with a boiling
point higher than the boiling point of the solvent otherwise they would be partially lost.
63
To minimize this effect, injection parameters as initial temperature of the injector, split flow rate
and duration of the split phase must be optimized .
To limit the loss of the most volatile substances, the injector temperature must be set at a value as
lower as possible during the split phase.
Fig. 59 - Solvent split injection: split and temperature profile
In some cases, the use of a cryogenic cooling of the injector is necessary.
If the presence of a small amount of solvent is acceptable, the duration of the split phase and the
split flow rate may be reduced, taking advantage of the refocalizing effect of the solvent (Solvent
effect).
Furthermore, the retention capacity of the injector insert can be increased by substituting the glass
wool with an adequate packing material, possibly coated with a stationary phase.
By optimizing the introduction conditions, a sample amount of up to 50-100 µl can be introduced

by this technique.
 To operate in Solvent Split mode open the page “Split” and at the parameter “Mode”
select “Solvent Split.”
64
Fig. 60 - Solvent split injection
Into the box “Split Flow” , set the split flow value, into “Split OFF” the time during the run at which
the “Split ” valve will be closed and in “Split ON the time at which the valve will be opened (fig. 60).
Pulsed introduction
When using the pulsed technique an higher inlet pressure is activated during the injection step for
a preset time.
Increasing pressure at the injection time helps to control expansion volume and improves transfer
of solutes to the column.
 To operate in this mode, it is necessary to set the inlet pressure at the injection time and
the duration of the pulsed pressure.
Open the page “Press/Flow” and press the button “Pulsed inj”. Insert into the boxes the values
and press ON to activate this mode. (fig. 61)
Fig. 61 - Pulsed Injection
65
When all setpoints are reached, the inscription “Prep” will appear in the “start” shortcut key and
“Stand by”in the Status bar. Pressing “Start” the pressure will increase up to the set value and in
the Status Bar the inscription “Ready” will appear.
Purge flow rate

As with the split/splitless injector, the PTV injector also has a purge line which provides a constant
flush of the introduction septum inside the injector. The purge line is fed by the same carrier gas as
the injector.
 To set the quantity of gas flowing into the purge open the page “Split” and press the button
“Purge”. Insert the value in the corresponding box (fig. 63).
Gas saving
The “Gas saving” is a special mode for saving the carrier gas through the reduction of split flow
during the analysis or when the GC isn’t utilized
 To set the value open the page “split” and press the button “Gas saving”. Press ON to turn
on
the gas saver flow and in the box “flow” insert the setpoint value.
The split flow rate will be reduced immediately, the “Stand by” status will be showed on the toolbar
and “Prep” will appear on the Start shortcut key.
Fig. 62 Purge flow rate Fig. 63 -Gas saving
In the box “Time” enter the time during the run when the split flow rate is reduced (fig. 62). In
case of split injection, set a time after the injection time. In case of splitless and/or pulsed
injection, set a time after the splitless or pulsed time.
Pressing “Prep ” will restore the initial split flow rate and “Ready” will be showed on the status bar .
66
Introducing the sample

Introduction of the sample at a low temperature prevents evaporation of the sample inside the
needle of the syringe.
This avoids sample discrimination and allows accurate measurement of the injected volume. In
general, therefore, the use of a syringe is not as critical as with the split/splitless injector. Since
the volume of the evaporation chamber is limited in order to promote thermal exchange, the
injection of small quantities is advisable in order to avoid over saturating the evaporator.
Higher quantities can be injected with the Solvent split technique (see Solvent split injection, in
this chapter).
When using the “Split” injection technique, the injection must be rapid and continue otherwise
double introduction phenomena can occur. If the splitless technique is used, therefore, the
carrier gas speed is lower, introduction must be slower but quite regular.
In case of “Solvent split” injection, the ideal introduction speed should correspond to the
evaporation speed of the solvent.
Since this is difficult to determine, it is advisable to carry out injection of the sample very slowly
(1µl/sec).
The slower introduction is carried out, the higher the injectable volume will be.
67
0
On Column – PTV
The capabilities of the PTV injector can be expanded to include true on-column injections
A new internal ring (fig 64) has been designed to allow to insert directly the syringe needle
(gauge 26) inside the column without a liner starting from a standard PTV injector.
Fig. 64 - On column - PTV: Internal ring
As shown in fig 65, this tool (1) must be screwed in the upper part of the PTV injector (in place
of the internal ring, spring and liner), then the septum (3) and the septum holder (2) have to be
positioned.
The internal restriction (4) allows to stop the column and align it to the syringe needle inlet . In
this manner the needle is guided inside the column with extreme precision.
At the moment the option On column-PTV is available for the application “Sim Dis” only.
How to install the column
Fig. 65 - On Column-PTV Injector
 Insert the column into the injector and partially hand screw the nut (5).
 Push the column upwards until the restrictor is reached and the column stopped.
 Using the pitch 7 spanner supplied, the nut should be tightened by 1/4 turn.
Avoid over tightening the nut since it could break the column
68
0
On column – PTV Injector: user interface
In order to control the On – Column PTV injector select “Menu”, “Tools” and then the injector B
o C depending on the configuration or by pressing the corresponding short cut key on the tool
bar.
Fig. 66 - On Column - PTV: User interface
The window “On-Col.\PTV (fig. 66) consists of five tabs: Temp, Press/Flow, Column, Split and
Status.
The parameters are the same of the PTV Injector and the only difference is the capability of
manage a columns of 0.53 of internal diameter. For further details you can refer to the PTV
injector Chapter.
69
0
Injector maintenance
Warning
Warning! The injector must be completely depressurized before doing any maintenance to
the injector.
Cleaning the precolumn

The precolumns of the split/splitless and PTV injectors request a periodic cleaning as they trap non
volatile compounds contained in traces in the samples and fragments of the injector septum.
It is not possible to define the duration of a precolumn as it depends on different factors as nature
of injected samples, number of injections, type and condition of the syringe needle.
Caution
Caution! The temperature of the oven, the injector and/or detector might be high
enough to cause burns.
To clean a precolumn proceed as follows:
• Remove the precolumn from the injector (refer to Assembling the precolumn in
the chapter headed Installing the columns ).
• Remove the glass wool.
• Wash the precolumn with a suitable solvent (ex. Hexane) to remove the residues on the
inner surface of the liner. During this operation, avoid to wet graphite seal.
• Prepare the precolumn as reported in the following paragraph.
Preparing the precolumn
Precolumn for Split/splitless injector

• With the aid a fine nylon thread (2), introduce the silanized glass wool (1) as illustrated in
the drawing herebelow. The glass wool should be 15 mm thick.
• Position the glass wool on level with the internal protrusion of the precolumn.
• Aspirate some solvent (e.g. Hexane) into the precolumn in order to clean the glass wool.
70
0
• Check that the graphite seal is adequately fixed to the glass and that the friction ring is in
place.
• Condition the precolumn in a stove at a temperature of 380 °C for 4-5 hours.
• Place the complete precolumn in the injector as instructed in the paragraph Assembling
the precolumn
SL/IN precolumn
Precolumn for the PTV injector

• With the aid a a fine nylon thread (2), introduce the silanized glass wool (1) as illustrated
in the drawing herebelow. The glass wool should be 20 mm thick.
• Position the glass wool at a distance of 3 mm from the lower end of the precolumn.
• Check that the graphite seal is adequately fixed to the glass and that the friction ring is in
place.
• Condition the precolumn in a stove at a temperature of 380°C for 4-5 hours.
• Place the complete precolumn in the injector as instructed in the paragraph,

Assembling the precolumn.
71
PTV precolumn
Precolumn for the PTV injector with adsorbent material

• With the aid a a fine nylon thread (2) , introduce the silanized glass wool(1) as illustrated
in the drawing. The glass wool should be about 5 mm thick.
• Position the glass wool at a distance of 20 mm from the lower end of the precolumn.
• Condition the precolumn in a stove at a temperature of 380°C for 4-5 hours.
• Let the precolumn get cold.
• Turn the precolumn upside down and fill it with the adsorbent material using a little
spatula. Use adsorbent material with fine granulometry (e.g. 80/100 mesh).
• Make this operation on a clean paper in order to recovery most of the material which
unavoidably does not enter the precolumn.
• Fill the precolumn with the material for about a 10 mm thick.
• Pack the adsorbent very well by beating the outside of the precolumn delicately.
• With the aid a a fine nylon thread , introduce the silanized glass wool in another
precolumn.
The glass wool should be about 5 mm thick.
72
• Position the glass wool at the level of one end of the precolumn.
• Place this end side by side with the end of the precolumn filled with adsorbent material.
• With the aid of a tubing with an outside diameter less than 1 mm (e.g. a piece of a wide
bore column), push the glass wool from one precolumn to the other.
In this way, the precolumn is filled with adsorbent material for a 10 mm thick, at a
distance less than 10 mm from the lower end.
The adsorbent material is blocked between two silanized glass wool plugs of 5 mm thick
each.
• Verify that the graphite ferrule is well fixed on the glass and the stainless steel washer is
present.
• Position the complete precolumn in the injector as described in the paragraph

“Assembling the precolumn” in the chapter “Installing the columns”.
Procedure for silanization of the precolumns

The following description is suitable for the silanization of precolumns for both the split/splitless
and the PTV injectors.
Proceed in the following manner:
• Prepare a solution of 5 % Dimethylchlorosilane in Toluene.
• Wet the inside of the precolumn with the silanizer, aspirating the solution with a
microbiological pipette connected with a silicone tube to the precolumn itself.
• If there is glass wool in the precolumn, it will also be silanized.
• Leave the liquid inside the precolumn for approximately 15 minutes taking care not to wet
the precolumn graphite seal with the silanizing solution.
• Eliminate the silanizing solution and wash the precolumn with Toluene, Methanol and
Diethyl Ether, in the said sequence.
Conditioning the split line filter

Pin-point the filter on the split gas line (see paragraph, Description, in this chapter).
• Disconnect both ends of the filter.
• Condition the filter in a stove at a temperature of 300°C for 4-5 hours.
• During conditioning the filter must be continuously flushed with Nitrogen or Helium at a
flow rate of 25-30 ml/min.
• A possible alternative is to open the filter and substitute the filling with 5A 60/80
molecular sieves
• In this case, the silanized glass wool balls, which are located at both ends of the filter,
should be substituted.
73
Detectors
• Reassemble the filter.
• Carry out the pneumatic leak test (see, Leak testing the pneumatic circuit, in the
chapter headed, Installing the columns)
Septa
The injector septa must be replaced periodically.
Substitution times are based on the number of introductions carried out and the quality of the
syringe. In fact, if the syringe is deformed, has snags or sharp angles the septum will suffer
damage and deteriorate more rapidly.
If the gas chromatograph is in constant use, if, for example, an automatic sampler is being used, it
is advisable to replace the introduction septum on a daily basis.
Important
Caution! The temperature of the injector might be high enough to cause burns.
Warning
When replacing the septum, the flow of carrier gas in the column is cut off. It is important
to allow the gas chromatograph oven to cool to room temperature before
proceeding with the above described substitution, since the capillary columns can
suffer damage if a high temperature is maintained in absence of the flow of the
carrier gas
Silicone septa must be washed and conditioned before use.

Washing procedure for the septa is described.
Washing procedure for silicone septa

• Place 10 septa in an Erlenmeyer flask.
• Add a solvent (e.g. Hexane) to the flask until the septa are completely immersed.
• As the septa swell, keep on adding solvent in order to maintain the septa completely
immersed.
• Leave to soak overnight.
• Eliminate the dirty solvent then rinse the septa with clean solvent.
• Eliminate the rinsing solvent.
• Dry the septa in a stove at a temperature of 80 °C until they return to their original
dimensions.
• Heat the septa at a temperature of 300°C for 12 hours.
Keep the septa in a clean, closed container.
74
Detectors
Procedure to close the Split/Splitless Septum holder
To properly close the septum holder of Split/Splitless Injector, proceed as the follows:
 Set the injector temperature at 50°C

 Screw the septum holder until it starts to offer a certain resistance (approximately two
turns). Do not overtighten the septum holder.
 Set the carrier gas pressure/flow parameters to the setpoint required by the method.
 In the page “Status” of injector, check if the pressure setpoint it reached and no alarm
of carrier gas pressure decrease is visualized.
 If the pressure set point is not reached or an alarm is present, it means that there is no
full sealing of injector.
 In the case, turn the septum further few degrees until no leakage is present and the
alarm disappears.
 Then, increase the injector temperature at the setpoint required by the method.
This procedure allows to close the septum holder when the temperature of the injector is low
and avoids the use to burn and following this procedure, the septum can be still easily pierced
without bending the needle.
It is always advisable to pierce manually the injector before starting a sequence with the
autosampler in particular mode for temperature higher than 300°C.
Split/Splitless injector cleaning procedure
The split/splitless injector might become dirty and active over time. In some cases you can solve
by changing the liner but, if this isn’t enough, a more vigorous cleaning procedure must be
performed.
The following procedure has been developed to help in this process.
The following parts and solvents will be needed:
 Hexane
 Acetone
 “Kimwipes”
 Spatula or stick
 Pliers
 Safety Glasses
 Lab coat
 Nitrile Chemical Resistant gloves
1. Cool the injector to 40°C selecting the value by the touch screen in the page “Inj X” tab
“Temp”
2. Cool Oven to 40°C selecting the value by the touch screen in the page “Oven” tab “Rate”
75
Detectors
3. Switch off the press/flow Control in the page “Inj X” tab “flow”, then switch off the GC
pressing the button on the GC front panel.
4. Remove the septum holder and then the internal ring with the suitable key.
5. Remove the spring and the liner from the injector with the pliers
6. Open the door. Loosen and remove the GC column nut from the inlet
7. Wrap the “Kimwipe” around a stick or a laboratory spatula (see Fig.67).
Fig. 67 – “Kimwipe” around a stick
8. Dip the stick in the hexane and insert it into the injector
9. Move it up and down and twist it on the bottom of the injector to clean all the internal
surface.
10. Remove the “Kimwipe” from the stick or spatula and wrap on another one. Move it up
and down inside the injector to remove the excess of hexane
11. Prepare another stick with the “Kimwipe” and dip it in the acetone.
12. Move it up and down and twist it on the bottom of the injector to clean all the internal
surface.
13. Switch on the GC and heat the injector to 80°C for 10 minutes to vaporize the solvent
away. THIS STEP CAN NOT BE BYPASSED
14. Reassemble the injector with a new liner with ferrule, spring, internal ring, new septa and
septum holder.
15. Install the column. Make sure that the column is re-cut prior to installation and use a new
ferrule.
16. Switch on the “Press/Flow Control” and check that the setpoint of the pressure is
correctly reached.
17. Heat the injector to the operating conditions, let it stabilize for 5 minutes. Make at least 2
blank runs before any analyte is injected.
76
Detectors
Detectors
In order to gain access to the “Detector” window, press Menu, Detectors, then A, B or C according
to the detector position.
You can also press the corresponding short cut key on the toolbar.
Flame Ionization Detector FID 86.10

Introduction
In the flame ionization detector (fig. 68), a microflame is produced at the nozzle outlet
when a Hydrogen flow comes into contact with a flow of air.
The nozzle and a coaxial steel tube form the electrodes of a circuit. A voltage is applied at each
end of this circuit.
Fig. 68 - Flame Ionization Detector

In normal conditions, the molecules of the pure carrier gas and of the auxiliary gas (if used) that
reach the flame are ionized and produce charges (positive and negative ions and
electrons): these charges, gathered by an electrode, generate a weak and constant current
called base current.
When an organic compound exits from the column and reaches the flame, through a
combustion process, the number of charges produced increases and subsequently the ionizing
current also increases.
The ionizing current passes through a resistor and generates a signal that is proportional to the
number of charges produced. This signal is adequately amplified and can be transmitted from
the electrometer to a registration system.
77
Detectors
The variation of the signal in time, caused by the passage of an organic compound through the
flame, determines registration of a peak.
The flame ionization detector has the characteristic of being highly sensitive to organic
compounds (10 - 100 pg according to the compound).
Sensitivity reaches a maximum with organic compounds containing Hydrogen, whereas it is lower
with organic compounds that have partially or totally oxidized carbon atoms (carboxyls,
carbonyl, alcohols, ...).
Some substances give low response or no response at all, amongst these: H2 O, CO, CO2 , SO2 ,
CS2 , Formaldehyde, Formic acid, N 2 , O2 , NH3 .
7
The FID detector gives an optimal linearity response, in the order of 10 times the minimum
sensitivity.
Description
The FID 86.10 detector can be used with both capillary and packed columns.
It is composed of three main parts:
• the base body

• the detector head
• the control unit
The base body

The base body (fig. 69) is composed of a stainless steel cylinder (1) welded to a support (2) and
secured to the gas chromatograph by two screws(3).
The unit is inserted into an aluminum block (4) containing the heating resistor (5) and the
temperature probe (6). Two gas lines are installed on the side of the base body:
• the inferior line (7) for the inflow of Hydrogen and auxiliary gases
• the upper line (8) for the inflow of air.
Fig. 69 - FID 86.10 base body
78
Detectors
A nozzle (9), which is electrically grounded, is screwed inside the base body. In the upper part, the
knurled brass ring (10) secures the head to the base body.
The end section of the body, inside the chromatographic oven, has a 1/4G thread (11).
Packed columns can be connected directly to this section with a 1/4G nut (12) and brass ferrules
(13).
If capillary or wide bore capillary columns are used, an adapter (14) to reduce the internal volume
of the base body should be installed: the end section of the adapter has a 4M thread.
The detector head

The detector head (fig. 70) is composed of :
• the electrode collector (1), coaxial to the nozzle
• the connector (2) to link up to the control unit
• the resistor for igniting the flame (3)
• the chimney (4)
Fig. 70 - FID 86.10 Head
The head is secured to the base body by a brass ring assembled on the base body.
An O-ring seal (5) inserted on the lower part of the head provides an adequate seal between the
head and base body.
The signal cable is connected to the connector (2) whereas the power supply cable is inserted onto
the flame ignition resistor connector (3).
Both cables come from the detector control unit.
The control unit

The control unit (fig. 71) provides electronic control of both the signal coming from the detector
head and the power supply.
The control unit includes an electrometer (1), the detector control board (2) and the resistor power
supply board (3) for igniting the flame.
79
Detectors
On the left side of the main board there is a connector (4) to link the control unit to the main board
of the gas chromatograph.
The signal cable (5), exiting from the electrometer, must be connected to the detector head; the
cable (6) supplies the igniter of the detector head.
Fig. 71 - FID control unit
Detector temperature
The base body temperature must always be set at a value that is higher than the maximum oven
temperature in order to avoid the condensation of the compounds in the line.
In any case it must be over 100°C in order to avoid water condensation.
Setting the temperature (“Temp” page)

The temperature of the detector can have a value between 40 and 450°C, with increment of 1°C.
Fig. 72 - FID Temperature
80
Detectors
 In order to set the detector temperature open the page “Temp”, press ON to activate the
temperature control and use the numerical keypad to insert the value in the corresponding box
(fig. 72).
Indication temperature (“Status” page)

 In order to see the detector temperature open the “Status” page. The number on the right
indicates the temperature set for the detector and on the left the actual temperature as measured
by the temperature probe (fig. 73).
Fig. 73 - FID Status
Regulating the gas flow rates

The sensitivity of the FID detector depends widely on the flow rate of the gases.
More particularly, the maximum ionizing results are obtained by optimizing the ratio between the
sum of carrier gas and auxiliary gas (if used) flow rates and the flow rate of the Hydrogen.
The carrier gas flow rate can vary considerably according to the type of column (packed or
capillary) and the separation.
With packed columns, once the flow rate of the carrier gas is established, the flow rate of the
Hydrogen will have to be optimized in order to obtain maximum response.
With capillary columns, since the flow rate of the carrier gas is reduced, an auxiliary gas flow must
be added. The optimal auxiliary gas is Nitrogen.
Response is higher with a Nitrogen/Hydrogen mixture than with a Helium/Hydrogen mixture.
In both cases, the ratio between the Hydrogen and the inert gas (carrier plus auxiliary) can be
optimized by regulating the auxiliary gas in relation to a constant Hydrogen flow.
In the FID 86.10 detector, for a Hydrogen flow of 38 ml/min, the optimal carrier and auxiliary gas
flow rate is 43 ml/min.
Air, which is the combustion support for the flame, must be available in stoichiometric excess
compared to the Hydrogen: under these conditions any flow variation will not influence the
ionization efficiency of the flame.
It is, therefore, advisable to work with flow rates higher than 300 ml/min.
81
Detectors
Setting the flow rates (“Flows” page)

 By opening the page “Flows” you can set all gas control parameters needed for the functioning
of the detector (fig. 74) .
Press ON to activate the flow controls and, through the drop-down menu, select the auxiliary gas
(Nitrogen or Helium).
Fig. 74 - FID Gas flow rates
By using the numerical key pad insert the gas flows rate values expressed in ml/min.
Aux and Hydrogen can have a value between 0 and 100 ml/min, with increment of 1 ml/min. The
setpoint of Air can range between 0 and 1000 ml/min, with increment of 1 ml/min.
Warning
Before regulating the Hydrogen flow rate, check that the detector is connected to a
column or protected by a closure in order to avoid the liberal escape of gas inside the
gas chromatograph oven this can cause explosion hazard
Visualizing gas flows (“Status” page)

In order to read the gas flow regulation open the “Status” page. The number on the right indicates
the set value and that on the left the actual value. (fig. 73)
Flame
In the page “Flame” you can find the following parameters (fig. 75):
• Flame threshold (mV): the FID produces a small signal current when lit.
This parameter defines the flame On condition. Master GC uses this value to determine
flame status (ON or OFF; see page “Status”) and controls the automatic re-ignition.
The flame will re-ignite if the signal drops below this value.
82
Detectors
This value, expressed in mV, can range between 0 and 1000 mV with increment of 0.01
mV.
• Auto Ignition: press “On” to enable the auto ignition function.
Fig. 75 - FID flame
Auto Ignition
Master GC is able to carry out an auto ignition procedure.
When the detector temperature reaches 200°C, the system starts the auto ignition procedure:
• the auxiliary gas (Aux) turns off and the Hydrogen is adjusted to 60 ml/min.
• the resistor for flame ignition switches on for few seconds . This process will cause a
small explosion.
When the flame is ignited, the signal level moves from 0 to a positive value.
Ignition can be checked by putting a cold shiny object near the chimney: condensation
will be present.
• the resistor switches off
• the auxiliary gas turns on and the Hydrogen is restored to the set point value
• the flame is checked to be “ON” (see “Status” page)
When the flame is “off”, the alarm “ FID FLAME OUT” will appear: the system will attempt to
re-ignite the flame up to five times at intervals of 1,5 minutes.
If the flame re-ignition fails, after 5 minutes the system turns off all FID gases and the alarm “FID
GAS CLOSED” will be shown.
Press “Clear” to cancel the alarm.
Signal
In order to set all the operative parameters for signal control, open the page “Signal” (fig. 76).
Selecting the RANGE level

The amplitude of the detector dynamic range can be varied to suit the analytic needs by selecting
the RANGE function.
83
Detectors
It means that, at different range, the same value of current measured by the detector produces a
different output signal.
84
Fig. 76 - FID Signal Fig. 77 - FID Range
Three range levels (1, 10, 100) are available: for each higher level, the dynamic range of the signal
produced by the detector is increased by a 10 factor compared with the previous level.
This results in a output signal 10 times lower for the same current value.
Set the RANGE function to 1 to get the minimum full scale range, that is the maximum sensitivity.
An example of the effect of the range on the signal is reported in the table below for both the 0-1
and 0-10 V scale.
Attention!
Do not use the scale 0-10V scale when you use the digital acquisition (LAN or USB)
Range Current Signal (0 - 1V) Signal (0 - 10V)
1 1 pA 1 mV 10 mV
10 1 pA 0,1 mV 1 mV
100 1 pA 0,01 mV 0,1 mV
Selection of the RANGE level depends on the analytic conditions: select the proper range level to
guarantee that all peaks of interest are within the detector dynamic range, which means that the
corresponding signal does not exceed the scale maximum and that at the same time they are not
too small to be correctly measured.
 Select the range levels through the drop-down menu (fig. 77).
85
Digital acquisition rate
As a general rule, at least 10-20 data for peak must be acquired to correctly define a peak.
This means that the acquisition rate must be select so that the product of Acquisition rate
(sampling/sec) and the peak width in seconds is between 10-20.
Besides, the response time provided by the electrometer must be adequate to detect fast peaks.
MasterGC provides two levels of response time: one for fast peaks (Min.Half-Peak Width < 0.6 sec)
and one for conventional peaks (Min.Half-Peak Width > 0.6sec). According to the Min. Half-Peak
Width setpoint (< 0.6 sec or > 0.6 sec), the response time will be automatically adjusted.
Digital acquisition rate (expressed in Hz) can assume the following values: 2.5, 10, 25, 50, 100,
250, 300.(fig. 88)
According to the Min.Half-Peak Width set, the optimal acquisition rate is automatically suggested .
You can still select a different one through the drop down menu.
Fig. 78 - FID Acquisition Fig. 79 - FID graph

rate
Graphic
In the page “Graph” the plot of the signal will be visualized. Use the buttons “+” and “-” to change
the time scale (expressed in minutes) and the Voltage scale (expressed in mV).
86
Electron Capture Detector ECD 86.10
Introduction
The electron capture detector (fig. 80) functions on the basis that electronegative substances
react with free electrons and form negative ions.
C + e-  C - + energy
The reduction in the quantity of free electrons is proportional to the concentration of the substance
and its electron affinity, that is, to its aptitude in capturing electrons.
The electrons are produced by ionizing the carrier gas with a radioactive source which produces �
particles.
This means that the flow of carrier gas from the gaschromatographic column, appropriately mixed
with the auxiliary gas, passes into an ionization chamber in which two electrodes are located.
63
The cathode, particularly, is a source of low energy radiation ( Ni): when the carrier gas exiting
from the column is introduced into the detector chamber, the radiation excites the gas molecules
producing ionization phenomena.
In this manner low energy free electrons and positive ions are formed.
When continuous current is applied to the two electrodes, because of the electrical field, the
charges move towards the electrodes of the opposite sign and generate a constant current in the
detector.
This current, appropriately amplified by an electrometric amplifier, is recorded as a constant base
current.
87
Fig. 80 - Electron Capture Detector
When a certain quantity of substance capable of capturing electrons is introduced into the
ionization cell, it becomes a negative ion and subtracts a certain number of electrons from the
system.
Consequently there is a reduction in the base current: this reduction, being proportional to the
quantity of substance and relative electron affinity, is used for a quantitative calculation of the
substance.
The system, as described, in which a constant voltage is applied to each end of the electrodes was
used in the first electron capture detectors which, in spite of a good sensitivity, showed a limited
response dynamic.
In most of the up-to-date devices, which include the DANI ECD 86.10, a variable frequency
impulse voltage is applied in order to maintain the current circulating in the circuit constant even in
presence of electron capturing substances.
Voltage is supplied with low frequency impulse, fo, during the passage of the pure carrier gas.
During the transit of an electron capturing substance, the circuit increases the frequency of the
voltage impulses, fc, in order to maintain the number of electrons in the system constant and
consequently the current in the cell.
The difference between the frequency when an electron capturing substance is present and the
initial frequency of the impulses (fc-fo) is measured: it is proportional to the concentration and to
the electron affinity of the substance under examination and represents the signal exiting from the
detector.
4
A detector with these characteristics guarantees a higher dynamic of linear response (up to 10 ).
In fact, the maximum efficiency of electron capture is obtained when the electron capturing
substances interact with “low energy” electrons.
However, because of the effects of the electrical field, the electrons are inevitably subject to an
acceleration which reduces the capture phenomena probabilities.
The supply of very brief impulse voltage limits the acceleration effect in that the electrons which
are not captured are periodically gathered around the electrodes and offers a better capture
efficiency even at higher concentrations.
The DANI ECD 86.10 detector is composed of a single body and the control unit.
88
The detector body
The detector body (fig. 81) consists of a stainless steel cylinder (1) assembled on a plate (2) which
is secured to the gas chromatograph by two screws (3).
The heating system is enclosed in an aluminum block (4) which contains the heating resistance (5)
and temperature probe (6).
The detector is equipped with an auxiliary gas line (7) which feeds gas just before the entry of the
ionization cell and mixes it with carrier gas.
Fig. 81 - ECD body
The vent line (8) on the upper part of the body connects the ionization cell with the
environment.
The ionization cell is located inside the detector body. It has a coaxial geometry: the collector
electrode (anode) is concentric to the ionization cell itself which consists of a stainless steel
cylinder connected to the ground (cathode).
63
The electron source consists of a plaque electroplated with Ni isotope held on the inside wall
ofthe cell.
The cell is electrically isolated by high temperature (400°C) resistant dielectric materials.
The anode terminal is connected to the control unit by a connector (10): the polarization voltage
supplied by the control unit reaches the electrode which in turn sends back the charges collected.
The lower part of the detector body ends in a threaded terminal (11) which goes into the
gaschromatographic oven.
The packed columns can be installed directly on the terminal by means of a 1/4G nut (12) and
suitable ferrules (13).
89
In order to install capillary or wide bore capillary columns a wide bore capillary column adapter
(14) that reduces the volume of the terminal and has a 4M threaded end must be applied.
The control unit

The control unit (fig. 82) provides electronic control of the detector.
The control unit is essentially a board (1) containing an excitation circuit that supplies variable
frequency voltage impulses, an electrometric circuit and a frequency-voltage converter (2).
On the left side of the main board there is a connector (3) for connecting the control unit to the
main board of the gas chromatograph.
Fig. 82 - ECD control unit
The control unit is located in the console of the gas chromatograph in one of the four positions
which are, from left to right, A, B, C and D and that correspond to the positions of the detectors.
The electrometer has an external cable with relative connector (4) for charge collection and
transmission of the excitation voltage.
Sensitivity and selectivity

The ECD is one of the most sensitive detectors used in gas chromatography. The detector
response to each single substance depends on the specific affinity of each one to the electrons.
The capacity to capture electrons varies significantly amongst the different substances (in a range
6
of 10 ) and depends on whether there are, or are not, electrophorus (atoms, groups or structures)
in the molecule.
Higher response is normally obtained from electronegative compounds containing halogens or

nitro groups.
For halogenated compounds, response decreases according to the sequence I> Br> Cl> F.
90
The table below provides, by way of indication, the relative response factor of several classes of
compounds:
Hydrocarbons 1
Ethers, Esters 10
Aliphatic alcohol, Ketones, Amines, mono-Cl 100

compounds and mono-F substitutes
mono-Br, di-Cl and di-F substitutes 1000
Anhydrides and tri-Cl substitutes 10000
mono I, di-Br, poli-Cl and poli-F substitutes 100000
di-I, tri-Br, poli-Cl and poli-F substitutes 1000000
Among compounds of the same kind, a small difference in the molecular structure can cause a
significant difference in response.
Sensitivity also depends on the position of the electrophorus and their number in the molecule.
o-Dichlorobenzene 42
m-Dichlorobenzene 30
p-Dichlorobenzene 11
-CHCl2 1
Response increases in a synergic manner with the increase in number of substitutions on the same
Carbon atom.
-CH3 , -CH2Cl 1
CH3Cl 2
-CHCl2 22
-CCl3 750 000
CCl4 11 300 000
91
The difference in response between compounds with different halogen/carbon ratio and mainly
the poor or lack of response of hydrocarbons in general make the ECD a detecting system which
other that being a sensitive system is also an extremely selective one.
This means that analyses results provide both quantity and quality information on the compound
of the sample analyzed.
On the other hand, it is precisely for this reason that a correct quantitative calculation always
requires the appropriate use of a calibration system.
Carrier gas and auxiliary gas

In order to produce free electrons, through ionizing radiation, it is essential to have a gas that is
easily ionized inside the cell.
Nitrogen and Argon at 5% Methane* are the most suitable gases and those most commonly used
in the electron capture detector.
They can be used either as carrier gas, more particularly with packed columns, or as an auxiliary
gas, for example with capillary columns, when added to the normally used carrier gas.
In both cases, whether the gas is carrier or auxiliary, it is important that the flow rate of the
Nitrogen or Argon-Methane reaching the detector is of at least 30-40 ml/min. Since the electron
capture detector is sensitive to concentrations, higher gas flow rates only lead to a reduction in the
detector’s sensitivity caused by increased dilution of the sample.
In order to obtain maximum working efficiency from the detector the carrier and auxiliary gases
should be extremely pure and humidity-free.
The presence of impurities, as for example H2O or O2 or any other electron capturing substance,
reduces the detector sensitivity in that any impurities take up some of the available electrons.
It is important to note that any type of leakage will also cause a reduction in sensitivity.
The cause of this is that through the leakage, environmental air sweeps into the detector and
subsequently into the cell. The presence of Oxygen in the air takes up electrons causing a
reduction in sensitivity. For the same reason, when there is a lack of carrier gas or auxiliary gas in
the detector for a certain period of time, Oxygen and humidity from the environment flow into the
lines and detector cell.
When the detector is re-activated it takes several hours to eliminate Oxygen and humidity and
restore optimal working conditions
*Methane, through deactivating molecular collisions, reduces the presence of metastable types of
Argon and reduces the energy of the electrons making them easier to be captured.
When the electron capture detector is in constant use, it is advisable to leave a continuous flow of
gas, even few ml/min, during the periods of inactivity (nights, weekends, etc.) keeping the
detector heating on and the gas chromatographic oven at a low temperature.
Setting the flow rate (“Flows” page)

 Open the page “Flows” (fig. 83) and press ON to activate the control flows: through the
drop-down menu, select the auxiliary gas (Nitrogen or Argon-Methane).
92
Insert in the box “Aux” the value required. The auxiliary flow can have a value between 0 and 100
ml/min, with increment of 1 ml/min.
Fig. 83 - ECD Aux gas

 In order to read the gas flow regulation open the “status” page. The number on the right
indicates the set value and on the left the actual value (fig. 84).
93
Fig. 84 - ECD Status page
Temperature
The response of the electron capture detector is highly influenced by the temperature of the
detector itself.
This is caused by the reaction mechanisms of the electrons with the molecules: some of these
mechanisms are aided by the temperature whereas others are inhibited.
Since different molecules have different reaction mechanisms, temperature effects are not the
same for all compounds. Therefore, it is fundamental that:
• the detector temperature remain constant.
• the detector temperature be always indicated particularly when sensitivity data is being
acquired (minimum detectable level) or the response of different compounds is being
compared.
The variation of response can reach three order of magnitude with a temperature difference of
250°C.
By optimizing the operating temperature response selectivity can be increased: by varying the
temperature the response of the particularly interesting compounds can be increased whereas the
response of the remaining compounds is decreased.
Compound Minimum detectable level (ppb)
80°C 227°C 350°C
CCl4 0.01 0.01 0.01
CHCl3 1.0 0.10 0.05
CH2Cl2 1000.0 40.0 8.0
CH2ClCH2Cl 1000.0 20.0 1.0
94
In any case the temperature of the detector must never fall below boiling point of the heaviest
compound of the sample under analysis and, when packed columns are in use, this is valid also of
the stationary phase.
It should, therefore, be sufficiently high so as to avoid condensation phenomena of heavy

substances inside the cell that could cause a significant reduction in sensitivity.
However, there is a temperature value which, when exceeded, may cause a high loss of
radioactivity: therefore, it is extremely important that the detector never exceed this limit.
It is for this reason that the ECD detector has a maximum temperature setting of 380°C.

 In order to set the detector temperature open the page “temp”, press ON to activate the
(fig. 85).
Indication temperature (“status” page)

 In order to see detector temperature open the “status” page. The number on the right indicates
the set oven temperature and on the left the actual oven temperature reading as measured by the
temperature probe (fig. 84).
95
Fig. 85 - ECD temperature
Current
 In order to set the detector current open the page “current”, press ON to activate the current
control and use the numerical keypad to insert the value in the corresponding box (fig. 86).
The current value can range between 0 and 10 nA, with increment of 0.001 nA
Fig. 86 - ECD Current
Signal
96
Fig. 87 - ECD Signal
250, 300.
According to the Min.Half-Peak Width set, the optimal acquisition rate is automatically suggested
(fig. 97). You can still select a different one through the drop down menu.
Signal zeroing
To zero the outgoing signal from the electrometer open the page “Signal”.
Insert in the box “Signal target” the signal level required and press “Apply”. The level will adjust to
meet the level required.
In the page “Status” you can visualize the signal and the back off (fig.84 )
The back off value, expressed in mV, represents the quantity added algebraically to the signal to
bring the signal level to the value set in the “Signal target” edit box.
Graphic
In the page “Graph” (fig. 88) the plot of the signal will be visualized. Use the buttons “+” and “-” to
change the time scale (expressed in minutes) and the Voltage scale (expressed in mV).
97
Fig. 88 - Graphic
Cleaning and conditioning the system

The electron capture detector is highly sensitive, therefore, the presence of impurities in the
system, contrary to other types of detectors, can cause problems.
In addition to the aforementioned pureness of the gas, all the other components of the detector
system require an elevated degree of cleanliness.
In particular, the introduction septa are a source of contamination which cannot be overlooked.
For this reason, it is important to follow the suggestions here below:
• use septa that are specifically for use with high sensitivity detectors and that are perfectly
washed and conditioned.
• keep the septa in a scrupulously clean and closed container.
• avoid direct handling of the septa during assembly by using a clean pair of pliers.
The analytic column must also be perfectly conditioned.

It is unadvisable to use columns that have stationary phases with poor stability or that contain a
high quantity of electro affined molecules, especially if the columns are of the packed type.
When turned on, the electron capture detector requires a relatively prolonged space of time (12-24
hours) in which to reach maximum efficiency level even when the columns are conditioned and the
pneumatic system perfectly clean. Conditioning is carried out with the detector at operating
temperature and with the presence of auxiliary gas.
A auto cleaning operation is carried out inside the ionizing cell, during this time: environmental
Oxygen and humidity, as well as any condensed substances inside the cell which, by taking up
electrons, reduce the efficiency of the detector, are eliminated through the combined effect of the
temperature and the passage of gas.
The practical effect of conditioning is that of a progressive reduction of the signal exiting from the
detector and, therefore, a progressive lowering of the base line, which indicates a minor presence
of electro-capturing contaminants inside the ionization cell.
98
In usual conditions, the base line is stable and the signal establishes itself on a minimum value: this
value corresponds to the minimum voltage impulse frequency required to maintain the set current
value when the system is clean and when pure gas is present.
Switching on the detector

To turn on the detector, the procedure is as follows:
• The detector conditioning requires a relatively long period of time (12-24 hours).
It is advisable to carry out this procedure from the night before the period of use.
• Start up the flow of auxiliary gas and set at least 15-20 ml/min flow rate value.
• Set the required operating temperature.
• After 12-24 hours, regulate the auxiliary gas (N2 or Argon-Methane) at 30-40 ml/min
flow rate. If the carrier gas is Nitrogen (or Argon-Methane), regulate the auxiliary gas
flow to obtain a total flow rate of 30-40 ml/min.
• Checking the signal, set increasing current values until the signal rises rapidly.
Allow a few seconds to elapse after each setting before checking the signal or base line
since the setting does not go into effect immediately. The rising signal indicates that the
detector is functional. Wait until the signal settles on a constant value.
The signal will usually settle on a value of about 10 mV .
Sometimes the value will be slightly higher. In this case, the current value can be lowered to
bring the signal to the indicated level.
Higher values indicate that the system is not sufficiently conditioned: detector sensitivity can be
nil or in any case highly reduced. If this happens, the conditioning operation should be
repeated with a higher auxiliary gas flow rate, if necessary.
• Once the detector is conditioned, regulate the auxiliary gas flow rate to the required
setpoint and turn on injector and oven heating.
At this point the signal might rise again: this is due to the elimination of residues from the
injector or the column.
When the column condition is completed, the signal will return to the initial level.
If packed columns are used, the signal will probably settle at a higher value that depends on the
oven temperature, the type of liquid phase in the column and the gas flow rate. It is evident that
the higher the level of the starting signal, the lower the sensitivity of the detector.
In this case, it is advisable to use operating conditions that minimize this effect on the column
and give a lower signal level (e.g. by decreasing the column temperature).
If in any case, even using capillary columns, the level of the signal remains higher than the
initial one or if it does not settle quickly, this indicates that the system is not clean. In this case,
check the injector (if necessary, change the pre-column) and/or thoroughly condition the
column, disconnecting it at the detector end.
When the conditioning procedure is carried out, the detector is ready for use.
If higher sensitivity is needed, set a higher current value but consider that, by doing so, the base
line noise also increases.
99
Usually, at maximum sensitivity conditions, the base line noise must not exceed 1% of the full
scale.
100
Detectors
Thermal Conductivity Detector TCD 86.40

Introduction
The thermal conductivity detector is based on the principle that a warm body undergoes a
temperature variation according to the thermal conductivity of the gas which surrounds it. The
temperature variation can be recorded and related to the gas concentration.
In the thermal conductivity detector, four metal filaments, inserted into the internal cavity of a heated
unit, are fed by constant current and, therefore, heated to a certain temperature. The filaments are
made of a metal which has an electrical resistance that varies significantly in relation to temperature
variations.
They are connected amongst themselves, in pairs, according to the Wheatstone bridge circuit (fig. 89).
The gas exiting from the analytical column (analytical channel) flows through one pair of filaments,
Fig. 89 - Wheatstone bridge circuit
whereas, pure carrier gas (reference channel) flows through the other pair.
When pure carrier gas flows through both channels, the two pairs of filaments S1, S2, R1 and R2 are at
the same temperature and have the same resistance value; the circuit is balanced and the signal exiting
from the detector is equal to zero.
When the component elutes from the analytical column, the thermal conductivity of the mixture of
carrier gas and component varies causing a corresponding change in the gas temperature.
The results is a variation in the electrical resistance of the filaments of the analytical channel while the gas
101
and electrical properties in the reference channel remain constant.
Consequently, an unbalance in the Wheatstone bridge occurs which produces an output signal from the
detector: this signal is recorded as a chromatogram.
The thermal conductivity detector is a non-destructive detector and, therefore, can be connected in
series with other detectors.
Description
The Thermal Conductivity Detector 86.40 is composed of the following principal parts:
• the main body and heating unit
• the external cover
The main body and heating unit

The main body (fig. 90) consists of a stainless steel block (1) inside of which there are four cells
(2). Each cell contains a filament in tungsten-rhenium (3), inserted by means of a seal system.
Each filament is connected to two wires (4). All the four filament wires are assembled in a single
cable which connect them to the control unit.
The filaments are connected amongst themselves according to a Wheatstone bridge circuit:
therefore, an analytical channel and a reference channel can be defined.
Each channel is connected at each end to a stainless steel tube with a diameter of 1.6 x 0.8 mm:
the inlet end (5) is connected to the column terminal, the opposite end is in direct contact with the
atmosphere (6).
The heating unit is located at the base of the main body (7).
102
Fig. 90 - TCD 86.40 main body
It contains an electric resistance (8) and a temperature probe (9) both of which are connected to
the gaschromatograph main board by a connector.
The external cover

The main body of the detector and the heating unit (fig. 91) are enclosed in a metal cover (1)
lined with insulating material which protects them from the external environment in order to
maintain a constant temperature.
The heating unit and main body are assembles on a metallic support (2): it has four lateral holes
(3) for securing the detector to the gas chromatograph.
The support has two 1/4G threaded ends (4) on which the packed columns can be directly installed
by using 1/4G fitting (5) and the brass ferrules (6).
Fig. 91 - TCD 86.40 external cover
To operate with wide-bore capillary columns, it is necessary to install an adapter (7) with a
lateral input for the auxiliary gas (8) and a 4M threaded end (9).
103
Two cables exit from the external cover: the upper cable (10) connects the filaments to the control
unit, the lower one (11) connects the electrical resistance and the temperature probe to the power
supply board of the gaschromatograph.
104
The control unit
The control unit (fig. 92) power operates the detector.
It consists of an electrometer (1) and the control board of the Wheatstone bridge circuit (2).
The wires coming from the detector head are connected to the terminal block (4).
Fig. 92 - TCD Control unit
Response
The response given by the thermal conductivity detector is expressed by the following equation:
R= ( )
where
K = constant based on the geometry of the cell

I = current of the filaments
Rf = resistance of the filaments
λg = thermal conductivity of the pure carrier gas at temperatureTb
λf = thermal conductivity of the sample
Tf = temperature of the filaments
Tb= temperature of the detector block
F = flow rate of the carrier gas
The factors which influence the detector response are analyzed here below.
105
Filament current
2
The term I in the above equation indicates that by increasing the value of the current in the
filaments, the response of the detector increases significantly. Moreover, an increase in the
current also corresponds to an increase in the temperature T f and the resistance R of the
filaments.
The result is that by redoubling the value of the current, a response which is from four to
eight times higher can be obtained.
The entity of the temperature increase of the filaments, and consequently of the response,
depends on the type of carrier gas and the temperature Tb of the detector block.
Therefore, a maximum current value must be respected in relation to the type of carrier gas
used and the detector temperature, otherwise there exists the risk of the overheating and
irremediable deterioration of the filaments.
It is advisable to operate using current values which are slightly lower than the maximum given
values (approx. 80%) in order to ensure higher stability of the base line and guarantee a
prolonged working life of the filaments.
The following table illustrates the maximum recommended current values according to the detector
temperature and the most commonly used carrier gases.
Detector temperature (°C) Carrier gas
He or H2 (mA) N2 or Ar (mA)
Ambient - 100 250 - 270 100 -120
100 - 150 220 - 250 90 - 110
150 - 200 200 - 220 80 - 100
Detector temperature (°C) Carrier gas
200 - 250 180 - 200 70 - 90
250 - 300 160 - 180 60 - 80
300 - 400 140 - 160 50 - 70
The current value in the circuit depends on the voltage value which feeds the filaments: it is, in
fact, the power supply voltage which is regulated in order to obtain the required current value.
Carrier and auxiliary gas

The detector response depends on the difference in the thermal conductivity of the pure carrier
gas and the gas containing the component to be detected: the higher the difference, the higher the
response will be for that component.
106
Thermal conductivity values of several gases are reported in the table below
Gas (0°C) (100°C)
Hydrogen 39.60 49.93
Helium 33.80 39.85
Methane 7.20 10.41
Oxygen 5.7 7.43
Nitrogen 5.66 7.18
Argon 3.88 5.09
Carbon Dioxide 3.38 5.06
Helium is the most recommended carrier gas since it has an elevated thermal conductivity value as
well as having the characteristics of chemical inertness and safety in use.
On the contrary, Helium is not the ideal gas for detecting Hydrogen in that the conductivity
difference between the two gases is minimum.
In this case the use of Nitrogen or Argon as carrier gas is more recommendable.
The use of Nitrogen will decrease the response factor in the case of Oxygen and Carbon Dioxide.
It is, therefore, evident that the choice of carrier gas must take into consideration various factors:
the components to be detected and their concentrations, the type of column, the safety conditions,
the purity of the gas available, costs, etc..
Since the detector response is influenced by the type of gas, it is advisable that the carrier and
auxiliary gas be the same.
Carrier and auxiliary gas flow rate

The TCD response is function of the concentration and therefore it is inversely proportional to the
total flow rate, that is the sum of carrier and auxiliary gas flow rates: the lower the flow rate, the
higher the response.
It is advisable that the sum of carrier and auxiliary gas flow rates be at least 20-25 ml/min.
Moreover, since the response is influenced by the flow rate it is indispensable that the total flow rate in
both the analytical and reference channels, be constant.
When operating in isothermal conditions, it is not strictly necessary that the flow rates be the same
but they must be constant.
It is, therefore, possible to install a different column or simply a restriction on the reference
channel.
Whereas, in the case of programmed temperature analyses the flow rates must necessarily be
identical because the variation of the flow rate with the temperature must also be identical: it is,
subsequently, indispensable that the columns on both channels be the same.
107
Temperature
The detector response is directly proportional to the factor (Tf-Tb), that is to the difference of the
temperature of the filaments and the temperature of the detector.
This means that the detector temperature must be set at a minimum value that is sufficient to
maintain the components in a gaseous phase, that is a value slightly higher than the boiling point
of the heaviest gas.
In case of isothermal analyses, the temperature should be equal to, or slightly higher than the
oven temperature; whereas, in the case of programmed temperature analyses, the detector
temperature should be equal or slightly higher than the temperature of the final isotherm.
To conclude, the TCD response can be increased by applying the following methods:
• by increasing the power supply voltage to the filaments
• by decreasing the temperature of the detector
• by optimizing the carrier gas
• by decreasing the gas flow rate to the detector.
108
Temperature

temperature control and use the numerical keypad to insert the value in the corresponding box .

 In order to see detector temperature open the “Status” page. The number on the right indicates
the oven temperature setpoint and on the left the actual oven temperature reading as measured
by the temperature probe .
Fig. 94 – TCD temperature Fig. 93 - TCD Status
109
Filaments
In order to control the filaments, open the page “Filaments” (fig. 95) and press ON. The
following parameters will be available:
• Voltage: it represents the power supply voltage on the filaments. This value, expressed in
V, can range between 0 and 20 V , with increment of 0.01 V.
If the pressure on Inj X or Aux X is too low, or an Injector used as safety haven’t been
configured, an alarm “FILAMENT SAFETY” will appear (ref. to table “Red Hand Alarm ” in
the chapter “Diagnostics”
Fig. 95 - TCD Filaments
• Polarity: it allows to set the polarity of the signal in order to have a positive signal.
• Max Current: this parameter, expressed in mA, represents the maximum current value in
relation to the type of carrier gas and the temperature of the detector. This value can
range between 0 and 300 mA, with increment of 1 mA. When the Current is over the Max
Current parameter, the alarm “TCD Voltage Reduced” will be displayed and the voltage
will be reduced (ref. to table “Red Hand Alarm ” in the chapter “Diagnostics”)
• Filament Safety: through the two drops down you can selected the injector or the gas
auxiliary used as Filament safety.
Signal

the RANGE function.
110
Fig. 96 - TCD Signal
Two range levels (1, 10) are available: at the higher level, the dynamic range of the signal
Selection of the RANGE level depends on the analytic conditions: they must be such, as to
 Select the range levels through the drop-down menu.

Digital acquisition rate (expressed in Hz) can assume the following values: 2.5, 10, 25, 50,
100,250, 300.
Signal zeroing
To zero the output signal from the electrometer open the page “Signal”.
Into the box “Signal target”, insert the signal level required and press “Apply”. The signal will
adjust to meet the level required. In the page “Status” you can visualize the signal and the back off
(fig. 94).
111
The back off value, expressed in mV, represents the quantity added algebraically to the signal to
bring it to the value set in the “Signal target” edit box.
Graphic
In the page “Graph” (fig. 97) the plot of the signal will be visualized. Use the buttons “+” and “-”
to change the value in time scale (expressed in minutes) and the Voltage scale(expressed in mV).
Fig. 97 - TCD Graphic
Switching on
In order to switch on the thermal conductivity detector the procedure is as follows:
• Prior to any operation the gas must flow into both channels.
See “Introduction Systems” values to set the required flow rate in the two channels.
• Set the oven temperature and the detector temperature. (See “Oven temperature” in the
chapter “Oven” and “Temperature” in this chapter)
Wait until the temperatures are constant, check that the base line is stable.
• In the parameter “Max Current”, set the maximum current value in relation to the type of
carrier gas and the temperature of the detector (ref. to table in “Current” paragraph and
“Filaments” paragraph of this chapter).
• In the parameter “Voltage”, set the value of power supply voltage on the filaments
(See"Filaments“ paragraph of this chapter).
Since each variation in voltage corresponds to a variation of the current and consequently a
variation in the temperature of the filaments, each time this parameter is modified, a pause is
necessary (30-60 mins) to allow the filaments to stabilize to the new conditions: in stable
conditions the base line must be constant.
112
Warnig
Each time the flow of gas to the detector is suspended, for example when replacing a column, an
introduction septum or on any occasion when the detector comes into contact with environmental
air, power supply to the filaments should be stopped. The presence of air can cause irremediable
oxidation and deterioration of the filaments.
• Check the detector functioning by reading under the parameter CURRENT in the
page “Status”, the value of the current in the circuit.
• Using the function “Polarity” set the polarity of the signal in order to have a positive
signal: this setting depends on which of the two channels will be used as analytical and
which as reference channel. (See"Filaments“ paragraph of this chapter
With reference to the above, it is important to observe that if a component, whose thermal
conductivity value is higher than the carrier gas, elutes from the column, the chromatogram will
show a negative peak (for example: Hydrogen with Nitrogen as a carrier gas).
113
Detectors
Nitrogen-Phosphorous Detector “Blos”
Introduction
The Nitrogen-Phosphorus detector (fig. 98) is a highly specific and selective detector for the
determination of traces of organic compounds Nitrogen and Phosphorus atoms in presence of
other organic compounds.
It consists of a collector and a jet similar to those of the flame ionization detector; the ion source,
instead, consists of a quartz bead containing a Rubidium salt, supported on a platinum wire and
positioned just over the jet.
During operation, negative ions are produced from catalytic interaction between the alkaline metal
and the compounds containing Nitrogen and Phosphorus.
Fig. 98 - Nitrogen Phosphorus Detector
The mechanism of this reaction is not completely known: the system is very complex and different
phenomena seem to be involved.
The gaseous environment inside the detector consists of a dilute mixture of Hydrogen in Air.
This mixtures is not able to maintain a ionizing flame and so the ionization of hydrocarbons is
negligible.
When the bead is fed with a negative voltage, the Rubidium salt contained generates ions; the
thermal energy produced by this heating forms a very reactive environment in the gaseous layer
surrounding the bead.
When substances containing Nitrogen or Phosphorus reach the reactive zone, they are
decomposed and ionized.
The negative ions formed by this reaction are gathered by a collector and the resulting current is
measured by the electrometer.
114
Description
The NPD Blos detector can be used with both capillary and packed columns. It is composed of
three main parts:
• the base body

The base body

secured to the gas chromatograph by two screws (3).
temperature probe (6).
Fig. 99 - NPD base body
Two gas lines are installed on the side of the base body:
• the inferior line (7) for the inlet of Hydrogen and auxiliary gases
• the upper line (8) for the inflow of air.
A nozzle (9), which is electrically grounded, is screwed inside the base body.
In the upper part, the knurled brass ring (10) secures the head to the base body.
Packed columns can be connected directly to this section with a 1/4G nut (12) and brass
115
The detector head
The detector head (fig. 100) is composed of :
• the electrode collector (1), coaxial to the nozzle

• the thermoionic source (2) supported on a platinum wire and fixed to the body by
a screw (3)
• the aluminum flange (4) which closes the inspection holes (5)
• the upper threaded lid (4) and the insulating mantle (7)
Fig. 100 - NPD Head
head and the body.
The signal cable is connected to the connector (9) whereas the bead power supply cable is
connected to the connector (10).
The control unit

The control unit (fig. 101) provides electronic control of both the signal coming from the detector
head and the power supply.
The control unit includes an electrometer (1), the detector control board (2) and the bead power
supply board (3).
On the left side of the main board there is a connector (4) for linking the control unit to the main
board of the gas chromatograph.
The signal cable (5) exits from the electrometer and the bead power supply cable (6) from the
bead power supply board.
116
Fig. 101 - NPD Control Unit
Sensitivity and selectivity

The NPD detector response towards molecules containing Nitrogen or Phosphorus is different for
different compounds and is difficult to predict.
Some compounds do not give any response to the NPD even if they have Nitrogen or Phosphorus
atoms (e.g. Nitro-glycerine) as it seems necessary a C-N bond to obtain a response.
The inorganic Nitrogen (e.g. N2 and NH3) is not determined as well.
The sensitivity and selectivity of the NPD are strongly affected by the flow rates of the gases and
the temperature of the thermionic source.
Effect of gas flow rates

A minimum change in the Hydrogen flow rate has a significant effect: in fact, the Hydrogen flow
rate affects the quantity of atoms of H in the reactive layer around the bead and in consequence
the detector response.
As the Hydrogen flow rate increases, the signal level and the response increase.
It is better to notice that when the response increases, even the baseline noise increases so that an
actual gain in sensitivity is not always obtained.
A very high flow rate has a negative effect as well as, as it can cause the flame ignition.
This condition brings to a loss in selectivity as the flame detects the presence of Hydrocarbons.
Furthermore, the flame damages the bead and reduces dramatically its working life.
The signal level and the response decrease by increasing the auxiliary gas flow rate. However,
the selectivity to the carbon compounds increases.
117
In any case, it is useful to observed that the sensitivity and the selectivity are inversely affected by
the gas flow rates so that these must be regulated differently in order to optimize one or the other
aspect.
Voltage to the bead

The voltage supplied to the bead causes its heating.
The ionization mechanism is activated by a threshold value.
By increasing the voltage over this value, the signal level and the response increase: even in this
case, when the signal increases the baseline noise rises too.
Therefore, it is better to evaluate at each condition the actual gain in sensitivity calculated as
signal/noise ratio.
Furthermore, as previously noticed, as the sensitivity increases, the selectivity decreases.
A progressive decrease in the sensitivity of the detector is normal and it is due to the gradual
consumption of the source.
The life expectancy of the bead is not predictable as it depends on the operative conditions: the
higher the power voltage and the Hydrogen quantity, the lower the duration of the bead.
Large quantity of chlorinated solvents and silanizing reagents damage the bead and reduce its
lifetime: therefore, it is advisable to eliminate as far as possible most of the solvent before the
injection.
The NPD detector is very sensitive to the presence of traces of contaminants which comes for
example from washing solutions of glassware or solvents.
Some stationary phases containing Nitrogen or Phosphorus (e.g. OV-225, OV-275, FFAP), columns
or glass wool washed with Phosphoric acid are not suggested as they can disturb the system.
Negative peaks can appear and they are caused by a rapid cooling of the bead (mostly due to the
solvent): normally, this problem is eliminated by increasing the bead voltage or the air flow rate.
Temperature
The temperature of the detector must be high enough to avoid condensation phenomena of the
substances in the sample.
Besides, the head temperature must be absolutely constant as it affects the bead temperature and
in consequence the sensitivity of the detector.
The insulating mantle helps to maintain the detector temperature constant.

temperature control and use the numerical keypad to insert the value in the corresponding box.
(fig. 102).
118
Fig. 102 - NPD Temperature

 In order to see detector temperature open the “status” page. The number on the right
indicates the set oven temperature and on the left the actual oven temperature reading as
measured by the temperature probe (fig. 103).
Fig. 103 - NPD Status
119
Regulating the gas flow rates

 By opening the page “Flows” (fig. 104), you can set all gas control parameters needed for the
functioning of the detectors.
Press ON to activate the control flows and, through the drop-down menu, select the auxiliary gas
type (Nitrogen or Helium).
Aux and Hydrogen can have a value between 0 and 100 ml/min, with increment of 1 ml/min. The
Air setpoint can range between 0 and 1000 ml/min, with increment of 1 ml/min.
Fig. 104 - NPD Flows
Warning
Before regulating the Hydrogen flow rate, check that the detector is connected to a column or
protected by a closure in order to avoid the liberal escape of gas inside the gas chromatograph
oven: this can cause an explosion.

In order to read the gas flow regulation open the “status” page. The number on the right indicates
the set value and on the left the actual value.
Bead
In order to set the value of the power voltage of the bead, open the page “Bead” (fig. 125).
Press ON and using the numerical keypad insert the value in the “Bead Voltage” edit box.
120
This parameter is expressed in V and can range between 0 and 1 V, with increment of 0.001 V.
Fig. 105 - NPD Bead
Detector functioning
• Set the detector temperature and wait till it reaches the required
value (see “Temperature” in this chapter)
• Set the carrier gas flow rate to the value required for carrying out the analysis
(see the chapter “Introduction systems”).
• Set the Hydrogen (about 3 ml/min), Air (about 60 ml/min) and auxiliary gas flow
rates (see “Regulating the gas flows rates” in this chapter)
• Select the Bead Voltage (see “Bead” in this chapter)
• Check the baseline at the “Status” page, on the acquisition system or on the
page “Graph” and set a progressive value of current until the signal level will
rapidly reach a positive value.
Wait some seconds between each set as the effect of the current on the signal is
slightly late.Wait until the signal stabilizes. These are the minimum operating
conditions.
The bead isincandescent and red.
Usually, a good bead starts working with a voltage between 0.550 and 0.700 V.
• Set a voltage value in order to obtain an output signal of about 10 mV.
Signal
In order to set all the operative parameters for signal control, open the page “Signal” (fig.106).
the RANGE function.
121
Fig. 106 - NPD Signal
122
250, 300.
Graphic
to change the time scale (expressed in minutes) and the Voltage scale (expressed in mV).
Fig. 107 - NPD Graph
123
Detectors
Flame Photometric Detector FPD 86.72

Introduction
The flame photometric detector (fig. 108) provides the selective determination of compounds
containing Sulphur and Phosphorus atoms.
The detector functions on the principle that compounds containing such eteroatoms produce
chemiluminescent species when burned in a Hydrogen enriched flame.
These molecules are produced in a metastable state and when they decay, they emit light of a
specific wavelength.
A photo multiplier measures and amplifies the light emitted.
Sulphur compounds are detected as the S=S molecules that emit light at 394 nm and phosphorous
compounds as the HPO molecules that emit light at 526 nm.
Fig. 108 - FPD Detector
An optical filter is installed between the flame and the photo multiplier to assure a high selectivity:
the filter has a band at 394 nm for sulphur compounds and at 526 nm for phosphorous
compounds.
When the light enters the photo multiplier, the electronics produce an output signal that is
amplified and can be send to the acquisition system.
124
Description
The FPD 86.72 detector can be used with both capillary and packed columns. It is composed of
three main parts:
• the base body

The base body

secured to the gas chromatograph by two screws(3).
temperature probe (6).
Two gas lines are installed on the side of the base body:
• the inferior line (7) for the inflow of Hydrogen and auxiliary gases
• the upper line (8) for the inflow of air
Fig. 109 - FPD 86.72 base body
A nozzle (9) is screwed inside the base body. In the upper part, the knurled brass ring (10) secures
the head to the base body.
125
Packed columns can be connected directly to this section with a 1/4G nut (12) and brass ferrules
(13).
If capillary or wide bore capillary columns are used, an adapter (14) to reduce the internal volume
of the base body should be installed: the end section of the adapter has a 4M thread.
The detector head
The detector head (fig. 110) is composed of:
• the combustion chamber (1) containing the upper nozzle coaxial to the nozzle of
the base body, a quartz cylinder blocked by a seal and a coated flange
• the chimney (2)
• the resistor for igniting the flame (3) and its connector
• the inlet for the Air 2 gas line (4)
• the photo multiplier (5)
Fig. 110 - FPD Head
A cable (6) for the feeding of the auxiliary heating exits from the detector head.
The photo multiplier is secured to the head by two screws (7) that is necessary to unscrew to
approach the filter (8).
Besides, a thermal filter is installed between the head and the photo multiplier.
The plugs to connect the signal cable (9) and the PMT power supply cable (10) coming from the
control unit, are at the end of the photo multiplier.
head and base body.
126
The control unit
The control unit (fig. 111) provides electronic control of the signal coming from the detector head
and the power supply of the flame resistor and of the photo multiplier.
Fig. 111 - FPD Control unit
The control unit includes an electrometer (1), the detector control board (2) and the boards that
controls the power supply to the flame resistor (3) and to the photo multiplier (4).
The signal cable (6) exits from the electrometer, the power supply cable for igniting the flame (7)
and the power supply cable for the photo multiplier(8) from the corresponding boards .
Gas flow rates

Sensitivity and selectivity are strongly affected by flame conditions that is by gas flow rates to the
detector. Particularly, the ratio Air/Hydrogen is crucial.
Furthermore, the optimal conditions are different if the Sulphur or the Phosphorus must be
determined.
The Sulphur determination requires a more reducing flame than Phosphorus that is a lower
Air/Hydrogen ratio: the optimal ratio is 0.6 for Sulphur and 0.8 for Phosphorus.
At a constant air flow rate, a Hydrogen flow rate increase increases the response up to a maximum
while the signal noise does not significantly increase; over this value the response decreases.
The selectivity towards hydrocarbons is lower with reduced Hydrogen flow rate.
Furthermore, the total flow rate of all the gases reaching the flame is important as it affects the
flame temperature.
The light intensity emitted by the chemiluminescent species, and the response as a consequence,
increases as the flame temperature decreases.
127
For this reason, it is advisable to use a gas with a high thermal conductivity as Helium or Hydrogen
as carrier and auxiliary gases instead of Nitrogen.
Using a 120 ml/min air flow rate at least, a total carrier and auxiliary gas flow rate of 20 ml/min is
enough to obtain a good response.

 By opening the page “Flows” (fig. 112) you can set all gas control parameters needed for the
functioning of the detectors.
Press ON to activate the control flows and, through the drop-down menu, select the auxiliary gas
(Nitrogen or Helium).
Fig. 112 - FPD Flows
Aux and Air can have a value between 0 and 100 ml/min, with increment of 1 ml/min. The setpoint
of air 2 and Hydrogen can range between 0 and 500 ml/min, with increment of 1 ml/min.
Warning
Before regulating the Hydrogen flow rate, check that the detector is connected to a column
or protected by a closure in order to avoid the liberal escape of gas inside the gas
chromatograph oven: this can cause an explosion
128
In order to read the gas flow regulation open the “Status” page. The number on the right indicates
the set value and on the left the actual value (fig.113).
Fig. 113 - FPD Status
The photomultiplier PMP

The detector response is strongly affected by the voltage which feeds the photo multiplier.
By increasing the voltage value, the response increases but at the same time the baseline noise
increases too.
The maximum sensitivity, expressed as signal/noise ratio, has been obtained with about 0.600 kV
for Phosphorus and about 0.650 kV for Sulphur determination.
 In order to set the voltage to the photo multiplier open the page “PMP” (fig. 114), press ON to
activate the PMP control and use the numerical keypad to insert the value in the corresponding edit
box.
The Voltage is expressed in kV can have values between 0.500 and 0.900 kV, with increment of
0.001 kV.
129
Fig. 114 - FPD - Photomultiplier
Temperature
The detector temperature affects its response as it affects the flame temperature.
Furthermore, as the flame is near to the photo multiplier, when the temperature increases the
baseline noise increases too.
Therefore, it is advisable to set the temperature high enough to avoid the condensation
phenomena keeping in mind that the response decreases with higher temperature.

The temperature of the base body can have a value between 40 and 450°C, with increment of
1°C.
 In order to set the base body temperature open the page “Temp”, press ON to activate the
(fig. 115).
To set the detector head temperature press “Menu”, select “Aux”, then open the
page“Temperatures” (fig. 116).
Insert the value in the corresponding edit box (see “Auxiliary temps and gases”).
130
Fig. 116 - FPD temperature Fig. 115 – FPD Aux Temperature
 In order to see detector temperature open the “Status” page. The number on the right indicates
the set oven temperature and on the left the actual oven temperature reading as measured by the
temperature probe .
Sulphur quenching
An undesired light absorption can occur in the flame when hydrocarbons and sulphur compounds
are analyzed in a mixture.
As a consequence, the response of Sulphur dramatically decreases.
This effect, called “quenching”, is due to the collisions that occur between sulphur species and CO2
molecules in the flame when a hydrocarbon at relatively high concentration coelutes with a sulphur
compound.
It is possible to reduce this negative effect by improving the chromatographic separation or by
using the detector in the double flame mode. The quenching effect can occur even at high
concentration of sulphur compounds (self quenching).This phenomenon does not occur with
phosphorous compounds.
Response factor
Due to the reactions of sulphur in the flame, the response of the Sulphur is not linear with the
concentration but is proportional to the square of the concentration, that is the square root of the
response is linear with the concentration.
The square root of the response is linear for 3 orders of magnitude.
131
The response of the Phosphorus is linear to concentration for about 4 orders of magnitude
values. (See “Temperature” in this chapter)
• Set the carrier gas flow rate to the value required for carrying out the analysis.
(See the chapter headed “Introduction systems”)
• Set the auxiliary gas flow rate in order to obtain a total flow rate (carrier gas +
auxiliary gas) of 20 ml/min at least.
• Set the Air 1 flow rate (4 ml/min)
• Set the Air 2 and the Hydrogen flow rate at different values depending on the
compounds to be analyzed (sulphur or phosphorous compounds).
Sulphur mode: Air 2 120 ml/min

H2 200 ml/min
Phosphorus mode: Air
ggen2 160 ml/min
H2 210 ml/min
Warning
Before regulating the Hydrogen flow rate, check that the detector is connected to a column
or protected by a closure in order to avoid the liberal escape of gas inside the gas
chromatograph oven: this can cause an explosion.
Igniting the flame
• Set the temperature of the base body and the head and wait until the reach
the required.
• Before igniting the flame, unscrew the detector cap.
• Open the page “PMP” and press ON to control the photo multiplier (the voltage
as default is 0.5 kV)The flame will ignite. This process will cause a small
explosion.The power voltage feeds the flame resistor for about 10 seconds and
successively feeds the photo multiplier.
• Screw the detector cap immediately after igniting the flame to avoiding the
room light entering the photo multiplier.
• Set the voltage to the photo multiplier.(see “Voltage to the photo
multiplier” in this chapter).Verify that the signal is positive in the page
“Status”.
Ignition can be checked by putting a cold shiny object near the chimney:
condensation will be present.
• Wait until the detector conditions stabilize.
• To operate in the double flame mode (ref. to the paragraph “Quenching of
Sulphur”) proceed in the same way and set the flow rates reported here
below:
Air 1 70 ml/min
Air 2 150 ml/min
Hydrogen 160 ml/min
132
• Optimize the flow rates according to the total gas flow (carrier gas + auxiliary
gas).
Fig. 117 - FPD Signal
Signal

the RANGE function.
133
250, 300.
Graphic
to change the time scale (expressed in minutes) and the Voltage scale (expressed in mV).
Fig. 118 - FPD Graph
134
Detectors
Micro-Thermal Conductivity Detector µTCD

Introduction
The principal of operation of the micro-thermal conductivity detector (fig. 139) is based on the
relative change in the thermal conductivity of the gas passing across the detector filament as
components elute from the column. Heat is lost continuously by the filament through the carrier
gas to the cell wall of the detector. A chromatographic signal is produced by measuring the amount
of current required to maintain the temperature of the filament constant when a gas with a
different thermal conductivity cross the filament. This process is non-destructive of the sample and
is concentration- dependent.
Fig. 119 - µTCD principle
The detector cell includes two separate filaments. Since changes in conductivity are measured only
by change in current required to keep the filament at a constant temperature, each of the two
filaments can be operated independently without referencing the changes to a match filament with
reference gas. This constant temperature provides longer filament life and safeguards it from the
extremely high temperature and oxidation which can occur with high concentrations of oxidative
or corrosive components.
The two filaments can operate in single or differential mode. The differential signal is provided to
minimize background variables such as column bleed and temperature programming.
Cell volume has been minimized to accommodate capillary column chromatography and optimize
the sensitivity of the detector at low flow rates. Carrier flow rates of 1-10 ml/min are recommended
for best sensitivity.
Each of the two filaments is controlled by a separate control unit which incorporated the
electrometer and the temperature control of the filament.
135
Description
The Micro Thermal Conductivity Detector is composed of the following principal parts:
• the detector cell and heater block

• two control units
The detector cell and heater block
The cell body and the heater block (fig. 120) are assembled into the detector housing and
protected by a housing cover. The housing is mounted on a metallic support secured to the
gaschromatograph by four lateral screws.
The detector housing contains an electric resistance and a temperature probe. Both of them are
connected to the gaschromatograph main board by a cable exiting on the right of the housing. A
cable on the left connects the filaments to the two control units.
The inlet lines installed into the detector are long enough to enter the column oven and permit
column connection. Each line is equipped with a fitting and a special adapter with a 4M threaded
end to directly connect the capillary column.
On the two side, the outlet lines of the two channels are available.
Fig. 120 - µTCD section view
The control units
The two control units are equivalent (fig. 121): they can operate independently to control the two
filaments in the single filament mode or can be linked through a dedicated cable (Part.No.
510.1509004) connected to the connector (1) to operate in the reference mode.
136
Fig. 121 - µTCD control unit
Each control unit consists of a main board (2) and a board for the filament and signal control (3) .
Each filament is connected to its control board by two of the four wires of the cable coming from
the detector head to the terminal block (5).
Configuration
In the configuration of the µTCD, two definitions for a channel (filament + control unit), “ µTCD”
and “ µTCD ref”, are available.
To operate single filament mode, configure both channels as “µTCD”; to operate in differential
mode, configure one channel “µTCD” and the other one “µTCD ref.”.
 In order to gain access to detector configuration, press “Menu” and select “Set up”. To open the
page “Det” you have to insert the password. (See the paragraph “Lock/Unlock” in the chapter “Set
up”)
Differential mode
In the differential mode, one channel must be configured as “µTCD”, one as “µTCD ref.” and the
control units must be connected through the proper cable.The two channels are independent for
all the functions except the temperature of the detector cell.
The sample should be injected in the channel named “µTCD”. In the differential operation, the
signal from the main channel is the actual signal produced by that channel while the signal from
the “µTCD ref.” channel is the difference (µTCD Signal - µTCD ref. Signal).
It means that, to acquire the differential signal, the signal coming from the “µTCD ref.” control unit
must be connected to the acquisition system.
137
 Select the “µTCD” and the “µTCD ref.” in the position (A and B) or (B and C) . The filaments
belonging to the same detector cell will be showed joined through a blue line (fig. 122 and 123).
Fig. 122 - A-B differential mode Fig. 123 -B-C differential mode
If you have two detector cells, the only configuration admitted is the following (fig. 124):
Fig. 124 - two det configuration
Single filament mode

In the single filament mode, the two control units are not connected and the signals coming from
the two control units are independent.
While operating in the single filament mode, carrier flow must be maintained to the non selected
filament, but it is not necessary to connect a column nor to apply any filament temperature.
138
To operate on both filaments, even simultaneously, both channels must be configured as “µTCD”.
Fig. 125 - A-B single mode Fig. 126 - B-C single mode
 Select the two “µTCD” in the position (A and B) or (B and C) . The filaments belonging to the
same detector cell are joined through a grey line (fig. 125 and 126).
If you have two detector cells the only configuration admitted is the following (fig. 127):
Fig. 127 - Two det configuration
Carrier and auxiliary gas

The detector response depends on the difference between the thermal conductivity of the pure
carrier gas and the gas containing the component to be detected: the greater the difference, the
greater the response for that component.
139
The table below shows the thermal conductivity values of several gases.
Gas (0°C) (100°C)
Hydrogen 39.60 49.93
Helium 33.80 39.85
Methane 7.20 10.41
Oxygen 5.7 7.43
Nitrogen 5.66 7.18
Argon 3.88 5.09
Carbon Dioxide 3.38 5.06
Helium is the most recommended carrier gas since it has a high thermal conductivity value as well
as the characteristics of chemical inertness and safety in use. On the contrary, Helium is not the
ideal gas for detecting Hydrogen as the conductivity difference between the two gases is
minimum.
In this case the use of Nitrogen or Argon as carrier gas is more recommendable.
On the other hand, the use of Nitrogen will decrease the response factor in the case of Oxygen and
Carbon Dioxide. It is, therefore, evident that the choice of carrier gas must take into consideration
several factors: the components to be detected and their concentrations, the type of column, the
safety conditions, the purity of the gas available, costs, etc..Since detection of low concentration
depends in part on the purity of carrier gas, to achieve the lowest possible detection limit the
highest carrier purity available must be used.
Carrier gas flow rate

The TCD response depends on the concentration: the lower the flow rate through the detector,
the higher the sensitivity .
The µTCD is designed for the low flow rates typical for capillary columns, and achieves best
sensitivity at rates below 10 ml/min. Since the filaments are maintained at constant temperature,
the detector can operate at extremely low flow rates (less than 0.5 ml/min) without damage to the
filaments.
Temperature
The detector response is directly proportional to the difference between the filament temperature
and detector temperature.
This means that the detector temperature must be set at a value slightly higher than the boiling
point of the highest boiling sample component and the filament temperature high enough to
achieve the desired sensitivity.
140
 In order to set the detector cell temperature open the page “Temp” (fig. 128) , press ON to
activate the temperature control and use the numerical keypad to insert the value in the
corresponding box.
Fig. 128 - µTCD temperature
Warning
It is advisable to increase the filament temperature step by step, for example 50, 80, 100 and so on
allowing each time the filaments to stabilize to the new conditions.
141
 In order to see the detector temperature open the “Status” page. The number on the right
indicates the temperature setpoint and that on the left the actual oven temperature as measured
by the temperature probe (fig. 129).
Fig. 129 - µTCD Status
Filaments
Single filament mode

In order to control the filaments open the page “Filaments” (fig. 130) and press ON.
142
Fig. 130 - Main Filament
In this way, the following parameters will be activated:
• Main Filament Temp: it represents the Main filament temperature. This value,
expressed in °C, can range between 40 and 400 °C , with increment of 1 °C.
If the pressure on Inj X is too low, or an Injector is selected as safety
which is not configured, an alarm “FILAMENT SAFETY MISSING” will appear
(refer to Table “Red Hand Alarm ” in the chapter headed “Diagnostics”
• Filament Safety: through the drop-down menu, select the injector used as
Filament safety.
143
Differential mode
In order to control the filaments open the page “Filaments” (fig. 131) and press ON.
Fig. 131- Main and Ref. Filaments
In this way, the following parameters will be activated:
• Main Filament Temp: it represents the Main filament temperature. This value,
expressed in °C, can range between 40 and 400 °C , with increment of 1 °C.
• Ref. Filament Temp: it represents the Reference filament temperature.

This value, expressed in °C, can range between 40 and 400 °C , with
increment of 1 °C.
• Main Filament Safety: through the drop-down menu, select the injector used as
Filament safety for the main filament.
• Reference Filament Safety: through the drop-down menu, select the injector
used as Filament safety for the reference filament.
144
Functioning
Once the detector has been installed, flow must be established prior to any heating of the detector
or filaments. Columns should be conditioned before connecting them to the detector.
Once conditioned, columns can be connected and flow established across both filaments.
Overall sensitivity increases as the difference between the filament temperature and the detector
temperature increases, but filament life decreases as its temperature increases.
Thus, the block temperature should be set as low as possible, with the ideal being just slightly
above the boiling point of the highest boiling component of the sample.
Allow adequate time for all temperatures to equilibrate as indicated by a stable baseline.
Typical equilibration time for block temperature from cold start-up to 130 °C is approximately one
hour. Detector block temperature changes take much longer to equilibrate than filament
temperature changes do.
Switching on
In order to switch on the micro thermal conductivity detector the procedure is as follows:
• Prior to any operation, the carrier gas must flow into both channels (see the
chapter headed “Introduction systems”)
The flow rates can be measured directly at the two exits, one on the right hand
side of the detector and the other one on the left.
• Set the oven temperature and the detector cell temperature. Wait until the
temperatures are constant. (see “Oven temperature” in the chapter “Oven”
and the paragraph “Temperature” in this chapter).
• Set the desired value of the filament temperature. Operating in the differential
mode, set the same for the other filament.
• When the filament temperatures are stable, proceed to the zeroing of the
signal as follows:
• Set the Main signal at a value slightly over zero (for example 5).To speed up
this procedure, it is advisable to set a higher value and then decrease it step by
step until the lower value is reached (see “Signal” in this chapter).
• Set the Reference signal in the same way. When both the Main and Reference
signals are near zero, the maximum dynamic range is obtained.
• In this condition, to obtain a positive signal the sample should be injected in

the Main channel.
• By injecting the sample in the Reference channel, a negative signal will be

produced.
145
• Besides, the baseline on the Reference should be set to a negative value until
a positive signal is obtained on the acquisition system.
Signal
In order to see all the operative parameters of the signal control, open the page “Signal” (fig.
132 and 133)
Fig. 133 - Signal single mode Fig. 132 - Signal diff. mode

Digital acquisition rate (expressed in Hz) can assume the following values: 2.5, 10, 25, 50,
100, 250, 300.
(fig. 132 and 133). You can still select a different one through the drop down menu.
Signal zeroing
To zero the output signal from the electrometer open the page “Signal” (fig. 152 and 153) .
Into the box “Signal target”, insert the signal level required for the Main and the Reference signal
and press “Apply”. The signal will adjust to meet the level required. In the page “Status” you can
visualize the signal and the back off .
The back off value, expressed in mV, represents the quantity algebraically added to the signal to
bring it to the value set in the “Signal target” edit box.
146
Graphic
In the page “Graph” (fig. 154) the plot of the signal will be visualized. Use the buttons “+”
and “-” to change the value in the time scale (expressed in minutes) and the Voltage scale
(expressed in mV).
Fig. 134 - Graph
147
Detectors
PhotoIonization Detector PID 86.90
Introduction
The photoionization detector (fig. 135) basically consists of a UV lamp and an ionization chamber. UV
rays pass through a Magnesium Fluoride window into the ionization chamber.
When the molecules of the compound absorb the radiation, a photo ionization process takes place
according to the following reaction:
Fig. 135 – Photoionization Detector
Inside the ionization chamber there are two electrodes to which a voltage is applied.
The electrically charged particles generated by the ionization process flow to the two electrodes
and produce a current. The current, which is proportional to the charges produced, is
subsequently amplified and measured.
Every compound is characterized by an ionization potential (IP): it represents the minimum energy value
of the radiation needed to ionize the molecules of that single compound.
The PID detector response is conditioned by ionization efficiency and, subsequently, radiation
energy. A weak response for a particular compound is caused by inefficient ionization which is in
turn caused by insufficient photon energy. As the lamp gives out photons with a constant
energy value, the response of the detector is conditioned by the ionization potential of each
compound and increases as their potential decreases: only the compounds with an ionization
potential which is equal or lower than the energy value of the photons can be efficiently ionized.
148
Compounds with higher potential will only be slightly ionized or not ionized at all and, therefore,
will give a weak response or no response at all.
There are UV lamps with different radiation energy: the most common are the 9.5, 10.2 and 11.7 eV.
The DANI PID 86.90 is equipped with a 10.2 eV lamp.
Description
The photoionization detector PID 86.90 is composed of :
• the base body

The base body
The base body (fig. 136) is composed of a stainless steel cylinder (1) welded to an aluminum support
(2) secured to the gaschromatograph by two screws (3). The body is inserted into an aluminum
block (4) containing the heating resistance (5) and the temperature probe (6). The auxiliary gas
line (7) is installed on the sides of the base body. A second line (8), which is usually closed, is
available in the case that the base body is used with other detector systems (e.g. FID, NPD, FDP). A
nozzle (9), which is electrically grounded, is screwed inside the body. In the upper part, the knurled
brass ring (10) secures the head to the base body.
Fig. 136 - PID base body
149
The end section of the body, inside the gaschromatographic oven, has a 1/4 G threaded end (11).
Packed columns can be connected directly to this end with a 1/4G nut (12) and the brass seals (13). If
capillary or wide bore capillary columns are used, an adapter to reduce the internal volume of
thebase body should be installed: the adapter has a 4M threaded end.
Detector head
The PID 86.90 detector head (fig. 137) has an upper part and a lower part which are screwed
together.
The upper part is composed of a nickel plated aluminum cap (1) that holds a UV light (2) held in
place by two brass semicircles (3). The light gives off radiation with 10.2 eV energy. The
radiation passes through a Magnesium Fluoride window (4) into the ionization chamber. The
power supply cable for the lamp exit from the aluminum cap (5) and has a Teflon connector (6)
on the other end.
The lower part is composed of a nickel plated aluminum body (7) covered inside by a Teflon
cylinder (8) on which an electrode collector is assembled; it contains a small glass cylinder (10) and
a Teflon seal disc (11): the ionization chamber is made up of these parts. Between the lower
and the upper parts there is a steel spring (12).
Fig. 137 - PID 86.90 Detector head
150
The body has a connector for link up to the control unit (13) and another for grounding the
detector (14); there is also a vent (15) for expulsion of gases from the ionizing chamber.
The connection between the base body and the head has an O-ring seal (16) positioned on the lower
extremity of the head.
The control unit
The control unit (fig. 138) provides electronic control of the detector.
The control unit includes an electrometer (1), a detector control board (2) and a board for the lamp
power supply (3). The power supply voltage to the lamp is about 600 V. The connector (4) for
link-up to the gas chromatograph is located on the side of the control unit.
The control unit is located in the console of the gas chromatograph in one of the four positions
which are, from left to right, A, B, C and D and that correspond to the positions of the detectors.
The signal cable (5) exits from the electrometer, the lamp power supply cable (6) and a detector
grounding cable (7) from the corresponding board.
Fig. 138 - PID 86.90 control unit
Temperature

 In order to set the detector temperature open the page “temp”, press ON to activate the
temperature control and use the numerical keypad to insert the value in the corresponding edit
box.
151
Fig. 140 - PID Status Fig. 139 - PID Temperature
 In order to see detector temperature open the “status” page. The number on the right
indicates the set oven temperature and on the left the actual oven temperature reading as
measured by the temperature probe.
Auxiliary gas
Setting the flow rate (“Flows” page)
 Press ON to activate the control flows (fig. 141) and, through the drop-down menu, select the
auxiliary gas (Nitrogen or Argon-Methane).
Insert in the edit box “Aux” the value required. The auxiliary flow can have a value between 0 and
100 ml/min, with increment of 1 ml/min.
152
Fig. 141 - PID Aux Gas
Visualizing gas flow (“Status” page)
 In order to read the gas flow regulation open the “status” page. The number on the right
indicates the set value and on the left the actual value.
Lamp
In the page “Lamp” (fig. 142) you can control the lamp. Press ON to turn on the lamp. Press
OFF to turn it off.
Fig. 142 - PID Lamp
153
Switching on the detector
• Feed the carrier gas and the auxiliary gas (if required). (see the chapter
headed “Introduction systems” and paragraph “Auxiliary gas” in this
chapter)
• Set the temperature of the base body at a minimum value that will avoid
condensation of low volatile substances from the sample or from the
column stationary phase. In most cases 150°C is more than enough.
In any case, the lamp will not withstand temperatures above 200°C.
It must also be considered that the higher the temperature, the lower
the life of the lamp (see “Temperature” in this chapter).
• Turn on the UV lamp (See “Lamp” in this chapter).
• Wait about 30 seconds for the set working conditions to stabilize (Check
the signal in the “Status” page).
Signal
In order to set all the operative parameters for signal control, open the page “Signal”.
the RANGE function.
Three range levels (1, 10, 100) are available: for each higher level, the dynamic range of the
signal produced by the detector is increased by a 10 factor compared with the previous level.
Set the RANGE function to 1 to get the minimum full scale range, that is the maximum
sensitivity.
154
Fig. 143 - PID Signal
250, 300.
Graphic
Fig. 144 - PID Graph

155
In the page “Graph” (fig. 144) the plot of the signal will be visualized. Use the buttons “+” and
“-” to change the value in the time scale (expressed in minutes) and the Voltage scale
(expressed in mV).
156
Auxiliary temps and gases
Auxiliary temperatures
In order to control the temperature of the auxiliary devices two Auxiliary temps are available. For
each Auxiliary seven control type can be selected.
Four of them have been optimized for the following devices:
Aux Oven: for the auxiliary Oven "Dani Master Aux"(cod 02111008600 )
FPD Aux: for the heating of the FPD detector head of the (See chapter Detectors
FPD)
ToF Tr. Line: for the heating of the Master ToF transfer line (TOF-MS detector cod
0317000100)
Union Heater: this device allows to heat the connection between the GC injector and
the transfer line of the autosampler (TD, SHS, DHS ecc)
Three further temperature controls are available in order to connect generic heating objects
with different thermal inertia: Aux temp Slow, Aux temp Medium and Aux temps Fast.
This control can be configured in "Set up" window "Aux" page and it is performed at factory or by
the DANI customer service engineer during the instrument installation.
 To enable the auxiliary temperature control open “Menu” and select “Aux”. In the page
“Temperature” the control modes Programmed or Oven Tracking can be selected.
Fig. 145 -Programmed Fig. 146 – Oven Tracking
157
In “programmed” mode (Fig. 145) you can set a single temperature and time “zero” to work at
constant temperature or insert a rate and/or a time to create a ramp of temperature.
In “Oven Tracking mode” (Fig. 146) the auxiliary temp can follow the Oven program.
The parameter Offset allows you to follow the Oven temperature maintaining a constant gap of
temperature.
The “Minimum temperature” represents the value from which the auxiliary temp is linked to
Oven temperature.
The temperature can be set from 30 up to 450°C with 1°C of increment. It is important to check
the maximum temperature reached to the connected device to avoid wrong settings.
Auxiliary gases
Three additional auxiliary gases control channels are available as an option . They are positioned
on the pneumatic department and identified as Aux 1, Aux 2 and Aux 3.
 This control can be configured in "Set up" window "Aux" page and it is performed at factory or
by the DANI customer service engineer during the instrument installation.
In order to set the parameters open "Menu" and select "Aux”. Every Auxiliary gas can be
controlled as flow or pressure mode. In the page "Press/Flow press ON to enable the Press/Flow
Control and select the control mode. (Fig 147)
Fig. 147 - Aux Gas - Control mode

.
In case of Control mode “Pressure” insert the pressure value in the table by using the numeric
keypad and press OK to confirm it. (Fig 148)
158
Fig. 148 - Pressure mode
The pressure can range from 0.01 up to 8.27 bar with 0.01 bar of increment
If the control mode is "Flow " insert the flow value in the table by using the numeric keypad and
press OK to confirm it. (Fig. 149)
The flow value can range from 0.1 to 100 ml/min
To allow the GC to work correctly in the selected mode, it is necessary enter the carrier gas type
and column dimensions in the page “Column”. (Fig. 150)
Fig. 149 - Flow mode Fig. 150 – Column
159
Method
Method
How to create a method

A method controls the functioning of the instrument during the analytical runs. To create a
method is necessary to specify several parameters:
• Oven temperature program (See the chapter headed "Oven"

• Injector parameters (See the chapter headed "Injection systems")
• Detector parameters (See the chapter headed "Detectors")
• Timed events (See "Timed Events" in this chapter)"
• etc..
It is possible to change some parameters during the analysis. In this case a pop-up "Confirmation"
will appear. Reply "Yes" to the question "Are you sure you want to change this setting during run?"
to modify the selected parameter.
Fig. 151 - Confirmation
When a parameter have been modified, an asterisk will be displayed on the right of the method
name.
Fig. 152 - Modified method
Pressing on the method name, the" Manage Methods" window will appear
This window contains two pages: the "Manage Methods" page and "Method Sequence" page.
160
Method
In the area of dialog "Active Method" of the "Manage Methods" page (fig. 153), you can find three
options:
Fig. 153 - Manage Method
to save the modification preserving the same name of the loaded method.
This function is active if:
• the current method has been modified

• The active method is different from the Default method.
to save the parameters entering a new method name. This key is active when:
• The instrument is not running

• There are no active sequences
• There is still some memory space to save the method
In order to enter a new method name an alphanumeric keypad will appear. Insert the name
and press OK to confirm. (Fig. 154 )
to create a new method starting from the Default method. This function is active if:

• There are not any active sequences
• There is still some memory space to save the method
All saved methods are listed in the frame "Stored Method" (fig 155).
161
Method
Fig. 155 – Kaypad Fig. 154 – Stored Methods
Pressing on the name of method you want to select, four options will be activated.
allows to load a method. This function is active if:

• If the current method has been modified and not saved, before loading the
selected method, the pop-up "Save Active Method" will open.
Replying "Yes" to the question, the changes to the current method will be
saved, answering "No" they will be lost.
Fig. 156 - Save Active Method
allows to copy a memorized method and to save it with a new name . This
key is activated when:
• There are still some memory space to save the method
162
Method
allows to eliminate a method. This function is active if:
• The instrument is not in running

Before deleting a memorized method a pop-up "Delete Method" will be displayed.

If you are sure you want to eliminate the method, reply "Yes" to the question.
Fig. 157 - Delete Method
allows to change the name of the method. The function is available when:

163
Method
Method Sequence
This paragraph contains the instructions to program a method sequence.
A sequence is a set of instructions for a range of runs. In this section you can only control the
Master GC and not the Master AS, so no sample will be injected. A method sequence can be useful
to automatize the instrument conditioning or the column cleaning.
In order to program a method sequence open the page "Method Sequence" (fig. 158), select a
method in the list "Stored Methods" and press ADD to insert it in "Method Seq.". You can enter up
to 25 methods and 50 repetitions for each method.
Fig. 158 - Method Sequence
When you select a method name in "Method Sequence" three functions will be activated:
• UP and DOWN: to modify the progressive order of the methods moving up or

down the selected method.
• REMOVE: to delete a method from the method sequence. If all methods are
deleted and the sequence is active, the message "NO ENTRIES IN METH.
SEQUENCE" will appear.
Press ON to active the sequence.
When a sequence is activated and the instrument is not in Ready condition, the inscription
AUTORUN will appear on the Start icon. (See Autorun in the chapter headed "Status and control of
analysis" ).
In this case. the sequence will start automatically when all the ready conditions are reached.
164
Method
Timed events
This paragraph explains how to automate signal, valve, and external events by programming in a
real-time clock (Clock time events) or during a run (Method Events).
Clock time events

Clock time events happen at certain time on specific days, based on a real time-clock. (See "Time
clock" in the chapter headed "Master GC user interface".
The following functions can be programmed:
• Load a method
• Start a method
• Start method sequence
• Start AS sequence
• Valve (opening and closing valve)
• External Events (Starting external events for other devices)
 In order to gain access to "Clock Time Events", press "Menu" and select "Timed Events". Open
the page "Clock time events" and press ON to enable the clock events.
Clicking "Add" the pop-up "Clock Time Event" will appear. Here you can select the event, the
parameter (for example the method name if the instrument must load a method or start a method,
etc..), the execution time and frequency. The Events available are listed in the table below.
Event Parameter
Load Method Method
Start Method Method
Start Method sequence
Start AS sequence
Valve Internal Event "n" ON "n": n. of valves installed (up to 4)
Internal Event "n" OFF "
External Events External event "n" ON "n": n. of external devices installed (up to 4)
External event "n" OFF "
165
Method
Use the box corresponding to "Execution time" to enter the time you want the event to take place,
based on 24-hour clock.
Fig. 159 - Clock Time Events Fig. 160 - Events programming
The programming event can occur:
• "ONCE": pressing on this box, a calendar will appear. Select day, month and
year you want the event to occur.
• "DAILY": the event will occur every day at the selected time.
• "WEEKLY": choose the day or the days of the week you want the event to
happen. Press OK to confirm the programming of the event.
All events are listed in the page "Clock Time Events". You can store up to 25 events. When you
select an event, the functions "MODIFY" and "DELETE" will be activated.
allows to modify the selected event. Pressing this button the pop up "Clock
Time Event" will appear. Make the changes and click OK to confirm.
allows to eliminate an event from the list. Pressing this button the pop-up
"Confirmation" will appear. Answer "Yes" to delete the selected event.
166
Method
Method events
You can program events to happen during a run (for example a valve can open three minutes into
a run). You can include a list of events for each analytical method.
The following events can be programmed:
• Range signal (see Detectors)

• Signal zeroing (see Detectors)
• Polarity change (see Detectors)
• Valve (opening and closing valves)
• External Events (events for external devices)
• Aux (see Auxiliary temps and gases)
 In order to gain access to "Method Events" press "Menu" and select "Timed Events".
Open the page "Method Events" and press ON to enable the events which occur at a certain point
during the analysis.
Method Events - Method Time Events
Clicking "Add", the pop-up "Method Time Event" will appear. Here you can select the event,
the parameter (for example the detector position if the instrument must carry out a signal
zeroing, etc..). The Events available are listed in the table below.
Event Parameter
Range Change Detector A, B or C 1X
Detector A, B or C 10X
Detector A, B or C 100X
Signal Zeroing Detector A, B or C
167
Method
Event Parameter
Polarity Change Detector A, B or C -
Detector A, B or C +
External Event External event "n" ON "n": number of installed external devices (up to 4)
External event "n" OFF "
Valve Internal event "n" ON "n": number of installed valves (up to 4)
Internal event "n" OFF "
Aux Aux Gas 1, 2 or 3 ON
Aux Gas 1, 2 or 3 OFF
Aux Gas 1, 2 or 3 Set Press
Aux Gas 1, 2 or 3 Set Flow
In the box "Executed at" enter the time (expressed in minutes) calculated from the start of the
analysis at which the event occurs. The setting interval allowed for each event is 0 - 999.00
minutes. Press OK to confirm the event.
All events are listed in the page "Method Events". You can store up to 40 events. When you
select an event the functions "MODIFY" and "DELETE" will be activated.
allows to modify the selected event. Pressing this button the pop up "Clock
Time Event" will appear. Make the changes and click OK to confirm.
allows to eliminate an event from the list. Pressing this button the pop-up
"Confirmation" will appear. Answer "Yes" to delete the selected event.
Fig. 161 - Confirmation
168
Status
Status
Instrument condition
The status of the instrument is shown on the Status Bar where the operative steps of the GC and
AS (if configured) are reported.
Stand by/Prep run
This condition indicates that the Oven and all the devices selected present are ready but their
values do not allow to carry out a correct analysis.
During this step, the Status bar will show the message “STAND BY” and the inscription “PREP” will
appear on the Start button.
Pressing “START/Prep ” Master GC will perform the following operation:
• When “Split” mode is programmed, PREP RUN is very fast and prepares the
system for the injection (Double start - see chapter Injection systems).
• When “Gas saving” function is programmed, PREP RUN ends the gas save
mode and resets the Split flow to the analytical flow. (see “Gas saving” in the
chapter headed “Injection systems”
• In “Splitless” mode, PREP RUN closes the split valve (see “Splitless” in the
chapter headed “Injection systems”
• In “Pulsed injection” mode, PREP RUN initiates the pressure increase (see
“Pulsed injection” in the chapter headed “Injection systems”
The instrument will remain in the “Prep run” condition until these parameters reach the initial
condition set in the method (see Ready conditions).
Ready
“Ready” indicates that the oven and all the devices selected as ready conditions (see Ready
conditions) have reached the values initially set for the method. The Status bar will show the
message READY.
The instrument can only accept the START command, whether keyed or remote, when all
conditions under “Ready” are present.
169
Status
Iso, Rate
When an analysis starts, the status bar continually shows the progress of analysis being carried
out. The display shows the step of the analysis in progress (number of isotherm or temperature
gradient) and time, in minutes and hundredths, which has elapsed since start.
Cooling
At the end of analysis, the oven cooling step is activated and the temperature is brought down to
the value set for the first isotherm. The status bar will show the message COOLING and the time
indication is active also during the cooling step. This means that an evaluation of the complete
analytical cycle can be made, calculated from the start of the analysis to the time when the
instrument reaches the Ready condition and, therefore, is ready for the next analysis.
Waiting
At the end of the cooling step, when the oven temperature reaches the value set for the first
isotherm, the instrument passes to the WAITING step.
During this step, the instrument waits for the oven to adjust, with extreme precision, to the
foreseen value.
The instrument will remain in the “Waiting” condition until the other parameters reach the initial
condition set in the method (See Ready conditions).
Conditioning
The conditioning step consists of an additional stabilizing time, calculated from the moment when
the instrument reaches the initial conditions. During this step, the Status bar will show the
message “CONDITIONING” and the time elapsed.
The duration of this step can vary from 0 to 999,00 minutes. To set this value select OVEN and
open the page General (see “Conditioning time” in the chapter headed “Oven”).
The Ready message will only show at the end of this step.
Autorun
When a sequence is activated and the instrument is not in Ready condition the inscription
AUTORUN will appear on the Start icon (see Method and Sequence in the chapter headed
“Method”).
170
Status
Pressing this shortkey, the GC passes in AUTORUN condition. In this case when all ready
conditions are reached, the sequence will start automatically
Control of analysis
Start of analysis
The analysis starts by pressing the button “START” positioned in the middle of the desktop or the
shortkey on the tool bar.
The START command determines commencement of all temperatures and pressures programmes.
The programmed time commands of “Method Timed Events” are carried out, according to analysis
time, calculated from the Start time (see Timed Events).
When a sequence of analyses or methods is activated, the Start command determines the start of
the sequence.
The Start command will only be accepted if the instrument is in READY condition.
If the instrument is not in Ready condition and a sequence of analyses or methods is activated the
inscription AUTORUN will appear on the Start icon.
Pressing this shortkey, the GC passes in AUTORUN condition (See Autorun in the chapter headed
“Instrument condition”). In this case, when all ready conditions are reached, the sequence
will start automatically.
End of analysis
The analysis will end automatically when the oven temperature program is finished.
However, the analysis can be stopped before completion of the program by pressing the STOP
button in the middle of the desktop or the shortkey on the tool bar.
Interruption of the oven temperature determines the interruption of any other program and the
reinstatement of all initial temperature, flow, pressure or timed event conditions.
Fig. 162 - End of analysis

171
Status
Before stopping the analysis, a pop-up will appear. Answering “Yes” at the question “Are you
sure?”, you confirm the stoppage of the analysis.
If a method sequence is in progress, the STOP command determines the stoppage of the
sequence: the instrument will return to the conditions of the first method of the sequence.
Fig. 163 - End of sequence
At the next START, the sequence will start from the first repetition of the first level.
lf you press STOP when a Master AS is installed and a sample sequence is running, a pop -up will
appear. Selecting "End analysis" the sequence will be stopped, but the analysis in progress will be
completed. Pressing ABORT both analysis and sequence will be interrupted).
172
Set up
Set up
The Master GC software controls all the parameters of the gas chromatograph: in order to carry out
correctly all the operative functions, the control unit must acquire all the information about the specific
configuration of each instrument. This task is performed at factory or by the DANI customer service
engineer during the instrument installation. Most of the set up parameters are accessible through a
password, and preferably managed by service people, to avoid unintentional modifications.
Only three pages, "Com", “AS” and "Other", are accessible to the final user.
Fig. 164 - Set up
 To gain access to "Set up" section, press Menu, Tools, then Set up.
Com
In this page (fig. 165) you can find all the parameters to connect Master GC to Clarity
software.
Activation code
To control Master GC through the Clarity or Empower software control driver, a specific code
must be entered in the "Activation code" box.
This code is strictly correlated to each DANI Master GC and it is reported in the Master GC
documentation provided with the instrument, only if a Clarity or Empower license has been bought.
173
Set up
Fig. 165 – Wrong activation code Fig. 166 - Communication
If the Activation code is not inserted or is wrong, a red message "Enter the right Activation code to
enable the communication with the Acquisition system" will appear (fig 165). In this case the
communication with Clarity software control driver is not enabled. This code is strictly correlated to
each license and is reported in the documentation provided with the software package.
Communication pipe
Master GC can communicate to a PC through three communication types: USB, LAN and RS232.
Besides, the analog output is available for all the detector signals.
Fig. 167 - Analog signal connections
 Select the communication pipe type through the drop-down menu.
• None: select this, if you use the signal analog output . In this case, connect the
signal cable to an external A/D converter or integrator according to the instruction
reported the figure below.
174
Set up
• Serial: This communication type provides a simple point to point communication. The
GC RS232 serial port 1 is connected to the PC RS232 serial port using a null modem
RS232 serial cable.
This type of communication has lower performance than USB and LAN and thus is
only provided as an alternative for situation where USB and LAN communication
are not applicable.
Fig. 169 – RS232 communication Fig. 168 - USB Communication
• USB: This is the easiest communication pipe to configure a point to point between PC
and Master GC. Please connect the USB cable only after the installation of driver on
the PC. The "USB device configured" message indicates that the Master GC is
correctly connected and is recognized by the PC.
Fig. 170 - LAN communication
• LAN: It's the most flexible communication pipe available for the Master GC.
According to your network configuration, LAN communication can be configured as
following:
175
Set up
Point to point: Suggest if you need to control only one Master GC to a PC.
You have to directly connect the PC network port to the Master GC network
porting using a LAN cross cable. (For TCP/IP configuration please see the
table below).
Server connection: Suggest if you want to take advantage of an existing

network infrastructure. Each Master GC has to be connected to the current
network HUB, SWITCH or RJ45 Ethernet wall plug using a LAN straight-
through cable.
Instrument network connection: Suggest if you need to control more the

one CG to a single PC. You have to connect the PC network port to a HUB
or SWITCH using a LAN straight-through cable. Each Master GC network
port has to be connected to HUB or SWITCH using a LAN straight cable.
(For TCP/IP configuration please see the table below)
Table: Suggested TCP/IP configuration for "point to point" connection and

"instrument network connection"
PC GC 1 GC 2 GC 3 GC 4
IP 192.168.0.80 192.168.0.81 192.168.0.82 192.168.0.83 192.168.0.84

Address
Subnet 255.255.255.0
mask
Default 192.168.0.1
gateway
176
Set up
Other
In this page you can find seven different items:
• Max Oven Temp: This parameter defines the maximum allowable oven temperature
setpoint to protect the column from damage. This limit must be set to the maximum
operating temperature recommended by the producer for that column.
• Cryo Oven: it allows you to configure the oven cryogenic system between liquid
carbon dioxide (Liquid CO2) or with liquid Nitrogen (Liquid N2).The oven
temperature range will change accordingly.
Fig. 172- Oven Max Temp Fig. 171 – Cryo Oven
• Pressure Unit: the pressure measurement unit can be selected. The measurement
units available are: bar, Psi or kPa. All set values will be automatically converted.
• Fast Oven cooling: This function is always active. In order to disable the fast cooling
press “OFF".
Fig. 173 - Pressure Unit
• Buzzer: select the buzzer ON to have a beep during an error condition.
177
Set up
• Ready In: this parameter allows to handle the incoming signal to Master GC (pin 7
and 8 Remote). You can select the functioning throughput drop down menu (Close
or Open) and modify the inscription in the box. This parameter, if set, can be a
ready condition and affect the GC status.
In order to set the "ready condition" and check the "Ready in status" press "Menu"
and select "Remote".
Fig. 174 - Ready In Fig. 175 - Ready In Status
• Ready Out: this parameter allows to handle the outgoing signal to Master GC (pin 3
and 4 Remote). You can select the functioning throughput drop down menu (Close or
Open)
Fig. 176 - Ready Out
178
Set up
• Start Only in Ready Status: Select this parameter in OFF to start the analysis even if
the GC status is not in Ready condition.
Attention!
It is not advisable to use this option if you are carrying out some quantitative analyses. To
start a measurement in not ready condition could give irreproducible results, affecting the
reliability of the analyses.
• GCXGC Mode: Select this parameter in ON when a Modulator for the GCXGC
technique is installed inside the Oven ( see the Chapter “Oven”).
Fig. 177 - GCxGC Mode
179
Set up
AS
This page allows to configure the Master AS by pressing the “ON” button.
Fig. 178- AS Set up Fig. 179 - SMPL
How to configure an external sampler
In case of an external sampler DANI (MasterTD, MasterDHS, MasterP&T, MasterSHS, etc) or other
devices that transfer the sample in vapor phase, it is necessary to flag the box corresponding to the
injector connected to the external sampler of the parameter “External sampling on”. (see fig 178)
In case of an external liquid sampler (HTA, CTC, etc), in addition to configure the parameter “External
sampling on” in the AS page, you have to flag the SMPL box near the injector connected to external
sampling in the page INJ (see fig. 179).
 In order to gain access to injector configuration, press “Menu” and select “Set up”. To open the page
“Inj” you have to digit the password.
Lock/Unlock
As described in the previous chapters, same pages are accessible only through a password. These
settings or functionalities are preferably managed by service people, to protect from unintentional
modifications.
The password will be delivered to the user only in special cases.
 In order to gain access to lock/unlock windows, press “Menu” , "Tools" then select
“Lock/Unlock”.
This window allows you to unlock or lock the pages covered by password and modify the
password. (Fig. 180)
180
Set up
Fig. 180 - Lock/Unlock
How to configure a cryogenic system for PTV injector

If a Cryogenic System is installed in the PTV injector you have to select the liquid utilized as a coolant
The minimum temperature reached are -50°C with liquid carbon dioxide and -100°C with liquid
nitrogen (see the “PTV injector” chapter)
When a PTV injector is configured the parameter “Cryo PTV” will be available (Fig. 181)
Fig. 181 - Cryo PTV
 In order to gain access to injector configuration, press “Menu” and select “Set up”. To open the page
“Inj” you have to digit the password.
181
Maintenance
Maintenance
The Maintenance window includes four pages to support the instrument maintenance.
Two of them are accessible only through a password, and preferably managed by service people,
to protect from unintentional modifications. The others two are available to the user for a routine
maintenance activity.
Fig. 182 - Maintenance
 To gain access to "Maintenance" section, press Menu, Tools, then Maintenance. The accessible
pages are: "Touch" and "Counters" (fig.182).
Touch screen calibration

In order to make the touch screen suitable to your finger touch, you can calibrate it.
 Open the page "Touch calib" and press the button "Calibrate touch screen". A series of circles
will be displayed. Press at the center of each circle (fig. 183).
At the end of this procedure the message "Congratulation, your touch screen has been calibrated"
will appear.
Press again the touch screen to continue.
182
Maintenance
Fig. 183 - Touch screen calibration
Counters
The usage of a gas chromatograph can cause some parts to get dirty or to be consumed.
These parts must be cleaned or changed periodically at a variable frequency, depending on the
number of analyses.
The page "Counters" can help in remembering the periodic maintenance, counting the number
of analyses from the last replacement of the parts.
The first and second section (Septum and Liner) increase only if the "Method sequence" is not
active. This means that they enhance only in case of real injection, thus in Manual injection or
when an AS Sequence is programmed.
Fig. 184 - Counters
Three columns are available:
183
Maintenance
• Name: insert the name of the device you want to monitor. Septum, liner and
column are already present as default but you can change them; two further
boxes are empty to insert others items.
• Threshold: defines the number of analyses (from 0 to 1000) after which you
should clean or change the part. As soon as the counter reaches this value, an
alarm will be produced.
Fig. 185 - Counter alarm
• Counter: shows the actual number of analyses occurred from the last
replacement.
When one counter exceeds its threshold, an alarm will be shown. In the "Alarm page" you can read
"COUNTER > THRESHOLD". This alarm still allows the instrument to reach the READY condition.
After replacement of the part, press the button "RESET" to reset the current counter and cancel
the alarm.
184
Diagnostics
Diagnostics
Diagnostic
When the instrument is switched on, a Self-test is performed to check the correct functioning of
the instrument. During this procedure, all the configured devices are checked one by one. At the
end, the diagnostic page will show all the devices in a list (fig. 186).
Fig. 187- Self test Fig. 186 - Self test alarm
If the device passes the test, a symbol "Ѵ" will be showed. If all the devices pass the self-test,
the Diagnostic window will close automatically and the desk top will be displayed.
If a device fails the test, an alarm (exclamation mark) will be visualized. In this case, at the end
of the self-test, the diagnostic page will remain open. Pressing on the device's name, a pop-up
will appear. Here detailed information about the device and/or the malfunctioning are
reported.
 To gain access to Diagnostic page press Menu, Tools and then Diagnostic.
The first item in the list is "System". Here you can read the serial number of the instrument and the
firmware version of the Main Board and the other controllers.
185
Diagnostics
Fig. 188 - System information
Alarms
When the control unit diagnoses an error condition, an exclamation mark, accompanied by an
acoustical signal (See “Buzzer” in the chapter "Maintenance"), will blink on the status bar near
the time clock.
This exclamation mark will flash till you click it or the condition which is causing the alarm remains.
Press the icon to display the "Alarms" page.

Here, the alarm message are listed. Press on the row: a pop-up will appear
containing details on the problem and, in most cases, the instructions to solve it .
Fig. 189 - Alarms
186
Diagnostics
Errors can be divided in:
• Parameters Error: these troubles spring from incorrect parameters you set. They will be
visualized by an hand near the message.
A red hand indicates an error that could cause serious damages. In this case
the START of analysis is blocked.
A blue hand indicates an error concerning a wrong setpoint. In this case the
START of analysis isn't blocked.
• Hardware Error: it indicates a malfunction of the instrument.
They are visualized by an exclamation mark. Pressing on the text a pop-up

will appear. It contains some details concerning the problem and, in most cases,
the instructions to solve it . The START of analysis is blocked.
In some cases, when you have solved the trouble, it is necessary to press "CLEAR" under the text
to bring the situation back to normal.
Fig. 190 - Alarm details
If the message shows " HARDWARE ERROR" you are invited to see the diagnostic page for
details. For these problems, it is preferable to refer to the technical assistance (see "Diagnostic" in
this chapter).
187
Diagnostics
BLUE HAND ALARMS
MESSAGE DESCRIPTION HOW TO SOLVE IT
NO ENTRIES IN METH. The method sequence is active but Insert a method in the sequence table
SEQUENCE the sequence table is empty. or deactivate the Method Sequence.
The active method will be used for (See Method)
the analysis
HIGH GAS SAVING The gas saving flow is higher than Modify gas saving flow. Gas saving
FLOW AT INJ X the split flow flow < split flow (See Introduction
To save gas the gas saving flow systems)
must be lower than the split flow
CRYO THRESH. < OVEN The cryo threshold is lower than Modify the cryo threshold. The
INIT. TEMP the oven initial temperature threshold value must be bigger then
The cryo will not be used to cool the oven initial temperature. (See
down the oven Oven)
CRYO THRESH. < PTV X The activation temperature of Modify the cryo threshold. The
INIT. TEMP cryogenic system is lower then the threshold value must be bigger then
PTV initial temperature. the PTV initial temperature. (See
The cryo will not be used to cool Introduction systems)
down the PTV
CLOCK EVENT(S) One or more clock event have not Check the parameters in the page
LOST(S) been executed because the GC was Timed events (see Method)
running or there was an error in Press CLEAR to delete the alarm
the event parameters
EVENT WITH EMPTY A "Start method sequence" event is Insert a method in Method sequence.
SEQUENCE programmed but the method (See Method)
sequence table is empty
Press CLEAR to delete the alarm
MODIFIED METHOD IN A modified method is included in Save the method (See Method)
SEQUENCE the method sequence. Running the
sequence the modifications will be
lost.
DET X: ACQ.FREQ. TOO Digital acquisition frequency for Modify the digital acquisition
LOW detector X is under the optimal for frequency or the Min. half peak width.
the set Min Half peak-width (See Detectors)
AS: RINSE VOLUME AS: Rinse volume higher than Modify the rinse volume
OVERFLOW syringe volume See (AS parameters in the chapter
Master AS)
AS:SOLVENT VOLUME AS: solvent volume is higher than Modify the solvent volume
OVERFLOW syringe volume See (AS parameters in the chapter
Master AS)
FID X FLAME OUT The flame of FID detector is out (See Fid in the chapter Detectors)
AS NEEDS AS needs calibration Check in Diagnostic (Autosampler)

CALIBRATION which injector or tray ref need to
calibrate.
See (How to align Master AS)
188
Diagnostics
BLUE HAND ALARMS
COUNTER>THRESHOLD One counter exceeded its (See Counters in the chapter

threshold. Maintenance) Reset the counter
for clear the alarm
OVEN RATE TOO HEIGH Oven temperature rate is not See Oven to set the correct rate
achievable in this temperature
interval
VIALS MISSING Vials were missing in the during See the chapter Master AS
last sequence. See details in the
Vials Tab
AS: SEQUENCE GC not ready at injection time Check for the parameter not ready
ABORTED at injection time. The cause could
be a wrong setting or a Master GC
problem.
189
Diagnostics
RED HAND ALARMS
OVEN: TEMP SET Oven temperature has been set higher than Insert a correct temperature
OVER MAX TEMP oven max. temperature setpoint
(See the chapter headed Oven)
OVEN Oven temperature unreachable without Turn the Cryo on or increase

TEMPERATURE cryogenic cooling. Please turn the cryo on or oven temperature.
UNREACHABLE increase oven temperature (See the chapter headed Oven)
PTV X PTV temperature unreachable without Turn the Cryo on or increase

TEMPERATURE cryogenic cooling. Please turn the cryo on or the PTV temperature.
UNREACHABLE increase PTV temperature (See Introduction systems)
INJ X TOTAL FLOW Injector Total flow is lower then 10 ml/min. Master GC can't correctly work
< 10 ML/MIN Please increase column flow,split flow or when total flow is lower then 10
purge flow. ml/min.
Modify the flows. (See
Introduction systems)
SPLIT ON TIME < Split on time is lower than split off time Set the split ON value superior
SPLIT OFF TIME then split Off value.
See ( Solvent split mode in the
chapter Introduction systems)
GAS SAVING TIME Gas saving time is lower that split on time Set the Gas saving time value
< SPLIT ON TIME superior than the Split ON.
See ( Introduction systems)
FIRST VIAL > LAST Sampler sequence first vial is greater than Insert the values correctly.
VIAL last vial. (see AS sequence in the chapter
headed Master AS)
NO ENTRIES IN AS The AS sequence table is active but empty. Insert the line in the table or
SEQ. TABLE deactivate the AS sequence.
(see AS sequence in the chapter
headed Master AS)
J.TCD REFERENCE A J.TCD Ref is configured without a linked (See Detectors)

FILAMENT main filament.
UNACCEPTABLE The detectors position configuration is (See Detectors -microTCD)

DETECTOR CONFIG. unacceptable.
AS VOLUMES The volume that will be taken in the syringe (See Set up in the chapter
OVERFLOW exceed the syringe volume. headed Master AS)
FILAMENT SAFETY Pressure on INJ X used as safety for (See Detectors)

filament is too low
FILAMENT SAFETY Pressure on AUX X used as safety for (See Detectors)

filament is too low
FILAMENT SAFETY Filament safety not selected (See Detectors)

MISSING
190
Diagnostics
RED HAND ALARMS
FILAMENT
MESSAGESAFETY Same filament safety selected for more than
DESCRIPTION (See Detectors) HOW TO SOL
DUPLICATE
RED HAND ALARMS one filament.
FID X GAS CLOSED The gas on FID X Detector has been closed Open the gas on fid and press
because flame was out. Clear in the "alarm" page to
cancel the alarm.
(See Detectors).
CRYO TIMEOUT Cryo save time elapsed. Cryogenic cooling (See Oven)
turned off.
CRYO FAULT Cryogenic cooling turned off. If the oven temperature doesn't
Oven cannot reach temperature set point. reach the set point by 16
minutes, the cryogenic system
will be deactivated
Checking the cryogenic system
(See Oven)
INJ X PRESSURE Calculated pressure for injector out of (See Introduction systems)
RANGE pressure range
INJ X FLOW RANGE Calculated flow for injector out of flow range (See Introduction systems)
INJ X SPLIT RANGE Calculated split for injector out of split range (See Introduction systems)
TCD VOLTAGE TCD filament current over max current. (See Detectors)
REDUCED Voltage reduced
AS: INVALID AS: One or more vial number present in See (AS parameters in the
VIAL IN sampler sequence are not valid chapter Master AS)
SEQUENCE
191
Diagnostics
HARDWARE ALARMS
OVEN TEMP. OVER Thermal shutdown: oven temperature oven Call the technical assistance
MAX TEMP. max safety temperature
INJ X PRESSURE Injector pressure decreased. Check for possible leakage.

DECREASED Oven temperature will be forced to 40°C for Then press "clear" to cancel the
safety and GC in splitless mode. alarm and restore the
introduction mode and the oven
temperature.
AS NOT FOUND The AS Sequence cannot be started. AS is Check for power supply cable or
not connected or not powered serial cable. (see Master AS
Sequence)
INJ X CARRIER Carrier gas pressure to Inj X is lower than Check the gas pressure
PRESSURE LOW required. available.
Oven temperature will be forced to 40°C for (See Introduction systems)
safety and GC in splitless mode. Press "clear" to cancel the
alarm and restore the
introduction mode and the oven
temperature.
HARDWARE ERROR Please see diagnostic page for details Generic hardware error.
See Diagnostics
192
Diagnostics
Leak test
In order to check for leaks in the carrier gas pneumatic system an automatic leak test have been
implemented.
This feature can be applied both the pneumatic system of the Master GC only and the GC with
autosampler ( for example Master GC + Master SHS or Mater GC + Master DHS) and it allows to
monitor the pressure on a "closed" system for 1 minute. There should be a loss no more than 0.3%
of the initial pressure.
 To perform the automatic leak test, press "Menu", "Diagnostic", open the "Leak test" page
then press the "Enter Leak test procedure" button. (Fig)
Fig. 191 - Leak test
• All the heated devices have to be at a constant temperature or, to avoid any
risk of burn, at room temperature.
• After turning off the detector gas control, disconnect the column from the
detector and seal the open end of the column. If no column is installed, close
the injector with the suitable plug (Cod. 2300303015).
• Select the position of injector then press "Next" (Fig. 192 )In this page, in
addition to the selection of the injector, the result of the last successful leak
test performed is visualized.
• After pressing "Next" the pressurization will start and it will be necessary
wait for the pressure equilibration to continue and press "Next". This button
will be activated only when the pressure is stabilized. The pressure value
reached is the inlet pressure (cylinder).
193
Diagnostics
Fig. 193 –Injector selection Fig. 192 - Pressurization
• During the leak test step the system is closed and the decrease of
pressure within 1 minute is monitored. If it is lower than 0.3% the leak test
will completed successfully.
Fig. 194 - Leak test in progress
194
Master AS
Master AS
The Master AS Automatic Liquid Sampler is an automatic sampler for the injection of liquid samples
into the Master GC.
It is mounted on the left side wall of the gas chromatograph and can inject into up to three
injectors .
It can operate traditionally using normal syringes for liquids.
Description
Master AS (fig. 209) includes:
• The moving block (1) consisting of three moving axes X, Y and Z. The
vertical axes Z includes the syringe housing and provide the vertical
movement of both the syringe and the plunger. The block moves along three
axes (X,Y and Z) to carry the syringe to the sample vials, to the solvent and
waste vials and to the injector A, B and C.A 160 sample tray for 2 ml vials
(standard) or a 65 sample tray for 10 ml vials (optional) (2). These removable
trays are seat in the base of the autosampler and blocked by the position
keys.
• A Solvent & Waste tray(3) that can contains up to five solvent or Internal
standard vials (10 ml) and up to five waste vials (10 ml). The tray is
removable, inserted on the base of the autosampler and blocked by the
position keys.
Fig. 195 - MasterAS
• The electrical connections are available on the back of the instrument.
195
Master AS
Syringe block
The syringe is lodged in an interchangeable support (1) and is held in place by a retainer (2). The
plunger head is set in an adjustable holder (3) and fixed by a blue screw (4). The syringe needle
is inserted in a retractable guide (5) protecting it from possible bends.
A transparent sliding cover protects the block (6) (fig. 196).
Fig. 196 - Syringe block
The electrical connections
The electrical connections, available on the back of the instrument (fig. 197) are: the supply
socket (1), the main switch (2), RS232 serial output (3) for the control of the instrument.
Fig. 197 - MasterAS connections
196
Master AS
Set up
The "Set up" window consists of two pages, "Vial & Syringe" and "Solv. & Waste", and allows you
to select the syringe volume, the vial dimensions and the position of Solvent, Internal standard and
Waste vials.
 To gain access to this section, press three times on the corresponding short cut key or select
"Menu", "Master AS" then "Set up".
Vial & Syringe
In the "Vial&Syringe" page, the following settings are available:
• Vial: select the vial type through a dropdown menu. (2 ml and 10 ml)
• Syringe: eight different syringes are available through a dropdown menu: 5,
10, 10 , 25, 50, 100, 250 and 500 µl).
Fig. 198 - Vial&Syringe

f
• Syringe Replacement: pressing this button the vertical arm of Master AS

moves to a useful position to replace the syringe (see "How to replace
the syringe" in the paragraph "Maintenance"). Press "Done" after the syringe
replacement: the vertical arm will move to its home position.
197
Master AS
Fig. 199 - Syringe Replacement
198
Master AS
Solvent&Waste
Master AS has got five positions, from A to E, for Solvent or Internal Standard vials and five
positions, from A to E, for the Waste Vials. In this page , you can select for each position if it will
contain a Solvent or an Internal Standard. You can also select if you want each Solvent and
Internal Standard wasted in separated vials or in the same vial (fig. 200).
Fig. 201 - Solvent Fig. 200 - Waste
AS parameters
 To gain access to this section you can press twice on the corresponding short cut key or select
"Menu", "Master AS" then "AS parameters".
Sampling mode (Inj. Mode)
Four sampling modes are available: Sample, Air Plug, Solvent Plug, Internal Standard.
The mode "Sample" is the standard injection mode: it can be combined with one or more other
modes to perform special injection techniques and take analytical advantages.
Sample
The syringe block moves to the sampling point, the needle enters into the vial and the plunger
moves up till measuring the sample volume selected in the method. In this mode, the needle
results full of liquid.
199
Master AS
In order to carry out a correct sampling, it is advisable to perform sample rinses and plunger
strokes (see "Sample Handling" in this paragraph).
In this case, before sampling, the syringe takes a selected volume of sample and discharges it into
the waste vial (Sample rinse). This operation is repeated several times according to the number set
in the method. To eliminate the air bubbles inside the syringe, the plunger moves up and down for
the number of times set in the method, keeping the needle dipped into the liquid.
 To select this injection mode insert the volume, expressed in µl (from 0.1 to 500), in the
"Sample" box.
The sample volume is shown in yellow on the syringe on the right of the display. The remaining
volume, in µl, is displayed on the top of the syringe.
Fig. 202 - Sample
If you set a sample volume higher than the capacity of the syringe, an alarm "AS volume overflow"
will be shown in the Alarm" page. The volume in excess is displayed on the top of the syringe.
Air Plug
The syringe block moves to the sampling point, the needle enters into the vial and, after rinses and
strokes (if selected), the plunger moves up till measuring the sample volume selected in the
method.
When the needle is out of the vial, the plunger lifts up to withdraw the volume of air plug set in the
method. By this way, the needle is full of air.
200
Master AS
Fig. 203 - Air Plug
 To select this injection mode press ON to active the "air plug" function. Insert the air volume,
expressed in µl (from 0.1 to 500), in the "Air plug" box and the sample volume in the "Sample" box
(fig. 203).
On the syringe on the right side of the display, the sample volume is shown in yellow and the air
plug volume in white. The remaining volume, in µl, is displayed on the top of the syringe.
If the total volume is higher than the capacity of the syringe, an alarm "AS volume overflow" will
be shown in the "Alarm" page. The volume in excess is displayed on the top of the syringe,
Solvent Plug
The syringe block moves to the “Solvent” position and both syringe and plunger move to take the
solvent.
After the syringe is withdrawn from the solvent, the plunger lifts up to take 0.5 µl air which will
separate the solvent from the sample.
Then, both the sample volume set in the method and air volume (if selected) will be taken.
In this way, a solvent plug is created which is separated from the sample by an air plug while a
second air plug fills the needle. During injection, the solvent plug improves the quantitative
transfer of the sample into the injector.
This mode does not allow to make any sample rinse and strokes.
 To select this injection mode press the "Solvent/IS Pos" to configure the position of the solvent
used as plug, then press ON to active the "Solvent Plug" function. Insert the solvent volume,
expressed
in µl (from 0.1 to 500), in the "Solvent plug" box and the sample volume in the "Sample" box.
201
Master AS
Fig. 204 - Solvent for "Solvent Plug"
On the syringe, on the right of the display, the sample volume is shown in yellow, the air plug
in white and the solvent plug volume in blue . The remaining syringe volume is displayed on the
top of the syringe.
If the total volume is higher than the capacity of the syringe, an alarm" AS volume overflow" will be
shown in the "Alarm" page. The volume in excess is displayed on the top of the syringe.
Fig. 205 - Solvent Plug
Internal Standard
After the syringe is withdrawn from the Internal Standard, the plunger lifts up to take 0.5 µl of air
to separate the IS from the sample.
202
Master AS
In order to carry out a correct sampling , it is advisable to set IS rinses and strokes (see "Sample
Handling" in this paragraph).
In this case, before sampling, the syringe takes a selected volume of IS and discharges it into the
waste vial (IS rinse). This operation is repeated several times according to the number set in the
method. To eliminate the air bubbles present inside the syringe, the plunger move up and down
keeping the needle dipped into the liquid.
Then, both the sample volume set in the method and air (if selected) will be taken. This mode
does not allow to make any sample rinse and strokes.
 To select this injection mode press the "Solvent/IS Pos" to configure the position of the I.S.
vial, then press ON to active the "Internal standard" function. Insert the solvent volume, expressed
in µl (from 0.1 to 500), in the "Internal standard" box and the sample volume in the "Sample"
box.
Fig. 206 - I.S. Configuration
On the syringe, on the right of the display, the sample volume is shown in yellow and the
I.S. volume in red (fig. 221). The remaining syringe volume is displayed on the top of the
syringe.
If the total volume is higher than the capacity of the syringe, an alarm" AS volume overflow" will
be shown in the "Alarm" page. The volume in excess is displayed on the top of the syringe.
203
Master AS
Fig. 207 - Internal Standard
204
Master AS
Sample Handling
Master AS is able to rinse the syringe with the sample or IS (if selected). In the "Sample Hand"
page the following parameters are available:
• Volume: this is the volume used for the sample rinse or IS rinse (if selected).
This value is expressed in µl and can range from 0.1 to 500 µl. If you set a
sample rinse volume or I.S rinse volume higher than the capacity of the
syringe, an alarm" AS volume overflow" will be shown in the "Alarm" page.
The sample or I.S. rinse will be wasted in the vial waste selected for the
"pre-solvent washing". If the "pre-solvent washing" is not selected ("none")
the sample or I.S. will be wasted in the Vial A.
Fig. 208 - Sample Handling
• Number: this value represents the number of repetitions (up to 25) for
sample or I.S. rinse.
• Sample Taking Height: It is the needle distance from the bottom of the vial
during the sampling. This value is expressed in millimeters and can range
from 0 to 30 mm.
• Plunger strokes: the plunger is able to move up at the speed set in "Plunger
speed (µl/s)" and down at a fixed speed. The strokes are very useful when
air bubbles are present inside the syringe. You can select up to 25 strokes.
• Plunger speed: This is the speed, expressed in µl/sec, at which the plunger
moves up. It can range from 0.1 to 100 µl/sec.
• Viscosity delay: it is the time, expressed in seconds, during which the
needle remains inside the vial before the injection. This function is important
when viscose solutions are sampled. This value can range from 0 to 25
seconds.
205
Master AS
Solvent Washing
The syringe washing can be performed at the beginning and/or at the end of each injection, with
the Pre Solvent Washing and the Post Solvent Washing respectively.
It is possible to use the same solvent both for the Pre-washing and post washing or two
different solvents in the two phases.
Fig. 209 - Solvent washing
To do this, the syringe block goes down on the solvent position, the syringe takes a set volume
of solvent and discharges it into the waste vial. This operation is repeated for the number of
washings with solvent set in the method.
The washing volume, expressed in µl, can range from 0.1 to 500 µl. If the washing volume is
higher than the capacity of the syringe, an alarm" AS volume overflow" will be shown in the
"Alarm" page.
The number of washings (up to 25) and the position of the solvent vial can be selected
separately for both the " Pre solvent Washing" and the "Post solvent washing".
206
Master AS
Injector
After taking the sample with one of the modes previously described, the syringe block moves to the
injector (A, B or C) selected. The block gets down and the needle enters into the injector at a
selectable speed and a selectable depth.
It is possible to check one or more injectors, if available. In this case, the sample will be injected
first in all the injectors in sequence then for all the repetitions included in the method (es.: sample
1: rep.1-inj.A/rep.1- inj B/rep.1-inj.C, rep.2-inj.A/rep.2-inj.B/rep.2-inj.C, etc..).
The needle can dwell into the injector for a certain time before injecting the sample (Pre Inj delay)
to perform the “Hot Needle” injection technique (see Introduction systems). A dwell time after the
injection (Post inj delay) can be also set in order to get a complete vaporization of the sample (fig.
210).
• Plunger Inj Speed: this is the speed of the plunger during injection: it is
expressed in (µl/s) and can range from 0.1 to 100 µl/sec.
Fig. 210 - Injector page
• Injector Needle Depth: It is the needle depth into the injector, expressed in
mm, and can range up to 45 mm.
• Pre Inj Delay/ Post Inj Delay: it is the time, expressed in seconds, during which
the needle remains inside the injector before the plunger lowers and after the
injection. It can range up to 25 seconds.
207
Master AS
AS Sequence
The "AS Sequence" window allows to set all parameters concerning the sampling sequence.
 To gain access to this section, press once on the corresponding short cut key or select "Menu",
"Master AS" then "AS Sequence".
How to create an AS sequence

Press Add to create a new row in the table : then, enter the position of the first and the last vials to
be sampled in the cell "First" and "Last" respectively.
Fig. 211 - AS Sequence
If the number of the first vial is higher than the last vial, the alarm "Last vial < First vial" will be
shown.
Specify the number of repetitions for each vial in the cell "Rep". The number of repetitions ranges
from 1 to 100. All the repetitions for the same vial will be processed before moving to the next.
208
Master AS
fig. 226 - AS sequence storing
Fig. 212 - AS Sequence storing
Clicking on the column "Method", all the stored method will be shown. Select the method to be
used for each sequence row.
Up to five different sequence can be stored as Sequence A, B, C, D or E according to the selection

on the dropdown menu.
In order to eliminate a line, click on the row to select it and press "Delete".
Press "ON" to active the sequence.
Fig. 213 - First AS Sequence Method
If the current Method is different from the first AS sequence method a pop up "Load First AS
Sequence Method" will appear (fig. 213).
Replying "Yes" the first AS sequence method will be loaded, selecting "No" the first method will be
loaded after pressing START.
209
Master AS
How to start an AS sequence

If an AS sequence is active and the GC is READY, press START once and the instrument will carry
out all the operations automatically.
If the instrument is not in Ready condition and a sequence is activated, the inscription AUTORUN
will appear on the Start icon.
Fig. 214 - Sequence Error
Pressing this short cut key, the GC will pass in AUTORUN condition (see "Status and control of
analysis"). The sequence will start automatically as soon as all the ready conditions are reached.
When the run is in progress, the ON/OFF button is disabled. In this case, a pop-up "Sequence
Error" will be shown.
How to stop a sequence

In order to stop a sequence, press the icon "Stop" in the toolbar or on the desktop. A pop-up
"Sampler sequence stop" will be shown : the sequence will pause to allow the selection among four
options:
• Resume: the sequence restarts from where it was stopped

• End Analysis: the current analysis ends, then the sequence stops
• Abort: the instrument stops both the analysis and the sequence
Fig. 215 - Stop a sequence
210
Master AS
• Abort & Wash: this option, active only during sampling, will stop the sequence
and wash the syringe with the solvent selected as "Post Washing Solvent".
AS status
The operating status of the Master AS is shown on the Status Bar by the indication
"SAMPLING".
Fig. 216 - AS Status
A detailed description of the AS status is available in the page "AS status".
In the upper frame "AS Status", all the steps are monitored in real time: Init. Sampling, Pre Solvent
Washing, Internal Standard, Solvent, Sampling, Air plug, Post Solvent Washing and Injection ( see
"Sampling mode" in this chapter).
In the lower frame "AS sequence", the number of set and actual repetitions, the method's name,
the vials and injector involved in the analysis are shown.
Missing vials
Before sampling, the syringe block moves to the position of the current vial and goes down to
check the presence of the vial.
In the AS status page, "Checking Vial" will be displayed.
211
Master AS
If the instrument does not check the vial, it moves to the next vial. An alarm "Vials missing " will be
shown. Details on the missing vials are reported in the page "Missing vials" that you can open by
clicking on the Status bar.
Fig. 218 – AS Missing Vial Fig. 217 – Priority Sequence
The table "AS Missing vial" consists of four columns and allows you to identify the missing vials,
the number of repetitions that have not been carried out and the method.
This feature is available only on Master AS equipped with vial presence sensor.
Priority Sequence
The "Priority sequence" allows you to setting up a sequence during the analysis. This sequence will
start immediately after the end of the current analysis.
 In order to program the priority sequence press the "Priority Seq" button. A pop- up will appear
(fig. 217).
Insert the first and last vial to be urgently sampled in the corresponding boxes, the number of
repetitions and the method to be used.
Press "On" to activate the Priority sequence control.
212
Master AS
Maintenance
To open the "Maintenance" window press Menu, select "Master AS", then "Maintenance"
(fig.
233).
Syringe Cleaning
This option allows you to manually wash the syringe.
Fig. 219 - AS Maintenance
Select the solvent through the dropdown menu "Position solvent" and insert the number
of washing in the corresponding box.
Pressing "Start", the washing procedure will begin.
During the Syringe cleaning, "SYR. CLEANING" will be reported both in the Status bar and in
the "AS Status" page.
To stop the syringe washing press "Abort"
213
Master AS
How to install the syringe

• Open the transparent sliding cover
• Keeping the needle guide completely lifted, insert the syringe into its seat by
inserting the needle through the holes on the seat and on the needle guide.
Keep the syringe with the graduated side frontally.
• Insert the syringe in the interchangeable support and the plunger head into its
seat on the adjustable holder and regulate the height by loosing the two
front screws, then fix the plunger head by the blue screw.
• Close the retainer to block the syringe.
• The standard syringe support is suitable for 5 and 10 µl syringes. For syringe
from 25 to 500 a different support is available as an option.
• To remove the syringe support pull it towards you. To install the other
support insert the four pins into the corresponding holes.
How to align the MasterAS

In order to align the Master AS referring to the TRAY position and the injector, selecting the
main MENU, “MASTER AS, then “MAINTENANCE” and follow the procedure
Alignment on the TRAY without the syringe (Z Axis)
• Press “Tray ref.” and wait until the vertical arm reaches the position set in
memory
• Select “ALIGNMENT” and use the appearing arrows (single arrow for slow
movements and double for fast movements) to move the arm along the Z
axis.
• Check the correct positioning by moving down the arm along the Z axis until
the needle guide touches the tray and the springs are released (See fig.)
Fig. 220 - Alignment on the tray position
214
Master AS
• Press STORE to memorize the position

• Select ZERO and press TRAY again to control the correct position. The
vertical arm will move only in the XY plane, select Z axis to verify the height.
Alignment on the Injector without the syringe
• Select INJ A (or INJ B or INJ C) and wait until the vertical arm reaches the
memorized position.
• Select “ALIGNMENT” and by using the arrows (single arrow for slow and
double for fast movements) move the arm along the X, Y and Z axes until
the septum holder conicity matches with that of the needle guide. The error
of one step in any direction due to human error or parallax error can be
tolerated.
Note: the needle guide must lean on the septum holder and the spring have
to be released.
• Press STORE to memorize.

• Select ZERO and press INJ A (or INJ B or INJ C) again to control the
position. The vertical arm will move only in the XY plane, select Z axis to
verify the height.
Alignment on the TRAY with the syringe (X-Y axes)
• Press “Tray ref.” and wait until the vertical arm reaches the position set in
memory.
• Select “ALIGNMENT” and use the appearing arrows (single arrow for slow
movements and double for fast movements) to move the arm along the axes
X and Y.
• Move the arm along X and Y axes till the tip of the needle is centered on the
CROSS drawn on the solvent/ waste tray. (See 201 ). The error of one step
in any direction due to human error or parallax error can be tolerated.
• Press STORE to memorize the position
Fig. 221 - Tray ref

215
Master AS
• Select ZERO and press TRAY again to control the correct position. The
vertical arm will move only in the XY plane, select Z axis to verify the height.
Checking the injector
• Select INJ A (or INJ B or INJ C) and wait until the vertical arm reaches the
memorized position.
• Press Z axis down arrow.
• Select “ALIGNMENT” and press slowly the single down arrow few times till
the syringe needle is totally inserted into the injector press CLEAR to escape
from alignment procedure.
Warning
At the end of the “checking the injector” you must not store the position, otherwise
you’ll memorize a wrong deep of injection and this could damage the Z axis.
216

MasterGC Operating Manual Rev.4.0

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MasterGC Operating Manual Rev.4.0

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A SCENT

MasterGC Gas Chromatograph

Rev. 4.0 (2014) from rev 20141003

Indicates a grounded terminal.

This symbol indicates a hot surface

Attention! Refer to attached documentation

Indicates hazardous voltages

Injectors and Detectors Compartment 3

Master GC User Interface 5

Installing the columns 24

PTV Injector (Programmed Temperature Vaporizer) 54

Flame Ionization Detector FID 86.10 77

Electron Capture Detector ECD 86.10 87

Thermal Conductivity Detector TCD 86.40 101

Nitrogen-Phosphorous Detector “Blos” 114

Flame Photometric Detector FPD 86.72 124

Micro-Thermal Conductivity Detector µTCD 135

PhotoIonization Detector PID 86.90 148

Auxiliary temps and gases 157

Auxiliary temperatures 157

How to create a method 160

Method Sequence 164

Timed events 165

Instrument condition 169

Control of analysis 171

How to configure a cryogenic system for PTV injector 181

Touch screen calibration 182

Leak test 193

Sample Handling 205

Solvent Washing 206

How to install the syringe 214

How to align the MasterAS 214

Operating temperature 0–40°C

LINE VOLTAGE REQUIREMENTS 240Vac (±10% max), 50-60 Hz, 3400 VA

Operating temperature 5°C above ambient to 500°C

Temperature setpoint resolution 1°C

Thermal accuracy ± 0.1°C

Thermal stability ± 0.1°C

Temperature programming 25 ramps, 26 isotherms, 0.1 to 140.0°C/min (see Table 1)

Typical cool-down rate 300°C to 50°C in 4 min

Isothermal time 0.00 to 999.00 min, 0.01 min setpoint resolution

Temperature 240V line voltage

Table 1 – Typical Master GC Oven Ramp Rates

Pressure range 0-120 psi

Carrier gas max total flow 1000 mL/min (He)

Pressure/flow programming Constant or programmed flow, constant or programmed

Atmospheric pressure and temperature

Injectors Packed (PK), split/splitless (SL/IN), programmable

Carrier gas He, N2, H2, Ar, Ar+CH4

Max number of PTV/ On column-PTV 2

Temperature Up to 450°C, 1°C setpoint resolution

Suitable for Capillary and wide-bore (0.53 mm i.d.) columns

Temperature Up to 450°C, 1°C setpoint resolution

Injection modes Split, splitless

Carrier gas control Digital flow control (DFC)

Liner Quartz liner with glass wool

PROGRAMMABLE TEMPERATURE VAPORIZER (PTV)

Suitable for Capillary columns

Temperature 10°C above ambient up to 450°C, 1°C resolution

Temperature programming 25 ramps, 26 isotherms

Heating rate 1 - 999°C/min; 1000°C ballistic

Injection modes Split, splitless, solvent split

Carrier gas control Digital flow control (DFC)